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Trifluoroacetic acid → HCID 86637595, 화합물

HRID 1694341
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반응식

HRID 1694341 반응식
C(OC([NH:8][NH:9][C:10](=[S:18])[C:11]1[CH:16]=[CH:15][C:14]([F:17])=[CH:13][CH:12]=1)=O)(C)(C)C.[F:19][C:20]([F:25])([F:24])[C:21]([OH:23])=[O:22].C1(SC)C=CC=CC=1>C(Cl)Cl>[F:19][C:20]([F:25])([F:24])[C:21]([OH:23])=[O:22].[F:17][C:14]1[CH:15]=[CH:16][C:11]([C:10]([NH:9][NH2:8])=[S:18])=[CH:12][CH:13]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6422Trifluoroacetic acidHCID 7520ThioanisoleHCID 866375961,1-Dimethylethyl 2-[(4-fluorophenyl)thioxomethyl]hydrazinecarboxylate

생성물 1

HCID 86637595HCID 86637595, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Trifluoroacetic salt. To a solution of N′-(4-fluoro-thiobenzoyl)-hydrazinecarboxylic acid tert-butyl ester (1.97 mmol) in CH2Cl2 is added trifluoroacetic acid (3 mL) and thioanisole (2.7 mmol). The mixture is stirred at room temperature for 1 hour. After evaporation of the solvent the mixture is purified by automated column chromatography (hexanes/EtOAc) to yield 4-fluoro-thiobenzoic acid hydrazide trifluoroacetic acid salt: 1H NMR (400 MHz, CDCl3) δ 9.5 (bs, 3H), 7.8-7.76 (m, 2H), 7.05 (t, J=8.4 Hz, 2H); LC/MS: (ES+) 171 (M+1)+.

후처리

  1. customAfter evaporation of the solvent the mixture
  2. customis purified by automated column chromatography (hexanes/EtOAc)

출처 및 근거

ORD 기록
ord-4ffe454f05bc4842b87275a51510b733
출처 데이터셋
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08158662B2

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