Piperazine, 1-(10,11-dihydro-2-fluoro-8-(1-methylethyl)dibenzo(b,f)thiepin-10-yl)-4-methyl-, methanesulfonate, hydrate (1:2:1)

Base Information

• Chemical Name: Piperazine, 1-(10,11-dihydro-2-fluoro-8-(1-methylethyl)dibenzo(b,f)thiepin-10-yl)-4-methyl-, methanesulfonate, hydrate (1:2:1)
• CAS No.: 91528-28-8
• Mol file: 91528-28-8.mol

Synonyms:

Chemical Property of Piperazine, 1-(10,11-dihydro-2-fluoro-8-(1-methylethyl)dibenzo(b,f)thiepin-10-yl)-4-methyl-, methanesulfonate, hydrate (1:2:1)

Chemical Property:

Purity/Quality:

Safty Information:

• Pictogram(s):  
• Hazard Codes: 

MSDS Files:

Useful:

Technology Process of Piperazine, 1-(10,11-dihydro-2-fluoro-8-(1-methylethyl)dibenzo(b,f)thiepin-10-yl)-4-methyl-, methanesulfonate, hydrate (1:2:1)

There total 12 articles about Piperazine, 1-(10,11-dihydro-2-fluoro-8-(1-methylethyl)dibenzo(b,f)thiepin-10-yl)-4-methyl-, methanesulfonate, hydrate (1:2:1) which guide to synthetic route it. The literature collected by LookChem mainly comes from the sharing of users and the free literature resources found by Internet computing technology. We keep the original model of the professional version of literature to make it easier and faster for users to retrieve and use. At the same time, we analyze and calculate the most feasible synthesis route with the highest yield for your reference as below:

synthetic route:

Reference yield:

4-mercapto-cumene (4946-14-9) → 1-(2-Fluoro-8-isopropyl-10,11-dihydro-dibenzo[b,f]thiepin-10-yl)-4-methyl-piperazine; compound with methanesulfonic acid (91528-28-8)

Guidance literature:

Multi-step reaction with 10 steps

1: 96 percent / KOH, Cu / H₂O / 1. 60 deg C, 15 min 2. reflux, 6h

2: 86 percent / sodium dihydrobis(2-methoxyetoxy)aluminate / benzene; toluene / 3 h / 40 °C

3: 91 percent / SOCl₂ / benzene / 2 h / Heating

4: 96 percent / ethanol; tetrahydrofuran; H₂O / 1. reflux 5 h 2. room temperature overnight

5: 83 percent / KOH / aq. ethanol / 6 h / Heating

6: 76 percent / polyphosphoric acid / 4.5 h / 150 - 155 °C

7: 92 percent / NaBH₄ / ethanol; tetrahydrofuran / 0.25 h / Heating

8: 87 percent / HCl, CaCl₂ / benzene / Ambient temperature; 1. saturation of solution with HCl gas, 4h 2. stand overnight

9: 90 percent / CHCl₃ / 7 h / Heating

10: ethanol / Ambient temperature; neutralization of INO 1730 with INO 1800

With hydrogenchloride; potassium hydroxide; sodium tetrahydroborate; thionyl chloride; PPA; copper; sodium bis(2-methoxyethoxy)aluminium dihydride; calcium chloride; In tetrahydrofuran; ethanol; chloroform; water; toluene; benzene;

DOI:10.1135/cccc19840086

Reference yield:

5-fluoro-2-iodobenzoic acid (52548-63-7) → 1-(2-Fluoro-8-isopropyl-10,11-dihydro-dibenzo[b,f]thiepin-10-yl)-4-methyl-piperazine; compound with methanesulfonic acid (91528-28-8)

Guidance literature:

Multi-step reaction with 10 steps

1: 96 percent / KOH, Cu / H₂O / 1. 60 deg C, 15 min 2. reflux, 6h

2: 86 percent / sodium dihydrobis(2-methoxyetoxy)aluminate / benzene; toluene / 3 h / 40 °C

3: 91 percent / SOCl₂ / benzene / 2 h / Heating

4: 96 percent / ethanol; tetrahydrofuran; H₂O / 1. reflux 5 h 2. room temperature overnight

5: 83 percent / KOH / aq. ethanol / 6 h / Heating

6: 76 percent / polyphosphoric acid / 4.5 h / 150 - 155 °C

7: 92 percent / NaBH₄ / ethanol; tetrahydrofuran / 0.25 h / Heating

8: 87 percent / HCl, CaCl₂ / benzene / Ambient temperature; 1. saturation of solution with HCl gas, 4h 2. stand overnight

9: 90 percent / CHCl₃ / 7 h / Heating

10: ethanol / Ambient temperature; neutralization of INO 1730 with INO 1800

With hydrogenchloride; potassium hydroxide; sodium tetrahydroborate; thionyl chloride; PPA; copper; sodium bis(2-methoxyethoxy)aluminium dihydride; calcium chloride; In tetrahydrofuran; ethanol; chloroform; water; toluene; benzene;

DOI:10.1135/cccc19840086

Reference yield:

5-fluoro-2-(4-isopropylphenylthio)benzyl chloride (91528-00-6) → 1-(2-Fluoro-8-isopropyl-10,11-dihydro-dibenzo[b,f]thiepin-10-yl)-4-methyl-piperazine; compound with methanesulfonic acid (91528-28-8)

Guidance literature:

Multi-step reaction with 7 steps

1: 96 percent / ethanol; tetrahydrofuran; H₂O / 1. reflux 5 h 2. room temperature overnight

2: 83 percent / KOH / aq. ethanol / 6 h / Heating

3: 76 percent / polyphosphoric acid / 4.5 h / 150 - 155 °C

4: 92 percent / NaBH₄ / ethanol; tetrahydrofuran / 0.25 h / Heating

5: 87 percent / HCl, CaCl₂ / benzene / Ambient temperature; 1. saturation of solution with HCl gas, 4h 2. stand overnight

6: 90 percent / CHCl₃ / 7 h / Heating

7: ethanol / Ambient temperature; neutralization of INO 1730 with INO 1800

With hydrogenchloride; potassium hydroxide; sodium tetrahydroborate; PPA; calcium chloride; In tetrahydrofuran; ethanol; chloroform; water; benzene;

DOI:10.1135/cccc19840086

upstream raw materials:

methanesulfonic acid

2-fluoro-8-isopropyl-10-(4-methylpiperazino)-10,11-dihydrodibenzothiepin

1-methyl-piperazine

4-mercapto-cumene