Reference

Chlorine-35 NQR and crystal structure studies of salts of chlorodifluoro- and dichloroacetic acid

Chlorine-35 NQR and crystal structure studies of salts of chlorodifluoro- and dichloroacetic acid. Basaran, Reha; Dou, Shi Qi; Weiss, Alarich (Inst. Phys. Chem., Phys.l Chem. III, Tech. Hochsch. Darmstadt, Darmstadt W-6100, Germany). Z. Naturforsch., A: Phys. Sci.Some commonly used reagents like 76-04-0 and 19740-21-7 are used in this experiment., 47(1-2), 241-50 (English) 1992. CODEN: ZNASEI. ISSN: 0932-0784. DOCUMENT TYPE: Journal CA Section: 77 (Magnetic Phenomena) Section cross-reference(s): 22, 75 The 35Cl NQR spectra of several chlorodifluoroacetates were studied as a function of temp., including the acid ClF2CCOOH. The cations were: ammonium, guanidinium, paramethylanilinium. Also some acid salts M+ClF2CCOO-.n-ClF2CCOOH (n 3 1) were studied by 35Cl NQR. The bleaching temps. of the NQR signals were detd. In the para-methylanilinium salt and in the guanidinium salt a phase transition has been obsd. The crystal structure of guanidinium chlorodifluoroacetate has been detd. at room temp. (a = 1089 pm, b = 845 pm, c = 832 pm, space group Pnma, Z = 4). For comparison, guanidinium dichloroacetate was studied by 35Cl NQR and by x-ray diffraction: P21/c, Z = 4, a = 804 pm, b = 1202 pm, c = 1080 pm, b = 131.58°. For guanidinium chlorodifluoroacetate and chlorodifluoroacetic acid, the 35Cl spin lattice relaxation time T1 and the line width have been followed up as a function of temp. Therefrom, the activation energies of the reorientation motion of the group-CF2Cl have been detd. to be 14 kJ.mol-1 (from T1) and 12.5 kJ.mol-1 (from Dv) for the pure acid and 9.2 kJ.mol-1 and 8.8 kJ.mol-1, resp., for the guanidinium salt. .

Preparation of organic 1,2-dichlorides with high selectivity

All Rights Reserved. Preparation of organic 1,2-dichlorides with high selectivity. Kaneko, YuJI (Fujifilm Holdings Corp., Japan). Jpn. Kokai Tokkyo Koho JP 2006348004 A 28 Dec 2006, 16pp. (Japanese). (Japan). CODEN: JKXXAF. APPLICATION: JP 2005-179887 20 Jun 2005. DOCUMENT TYPE: Patent CA Section: 23 (Aliphatic Compounds) YACR1R2CR3R4(CR5R6)mCHClCH2Cl (Y = alkyl, aryl, acyl, alkoxycarbonyl; A = O, S, NR; R = C1-5 alkyl; R1-R6 = H, C1-5 alkyl, C1-5 alkoxy; n = 0-3) are prepd. by chlorination of YACR1R2CR3R4(CR5R6)mCH:CH2 with Cl in the presence of chlorination accelerators, preferably radical scavengers. 881903-14-6 and 76-04-0 which are cas registry numbers of substances are two of reagents here. Thus, F2ClCCO2CHEtCH2CH:CH2 (prepd. from EtCHO, CH2:CHCH2Br, and F2ClCCO2H) was chlorinated with Cl in the presence of pentaerythritol tetrakis(3,5-di-tert-butyl-4-hydroxyhydrocinnamate) to give 93% F2ClCCO2CHEtCH2CHClCH2Cl. .