Trifluoroacetic acid → HCID 86684904, 화합물

HRID 2402895노트

반응식

HRID 2402895 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[SH:9].FC(F)(F)C(O)=O.[C:17]1([C:23]([C:31]2[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=2)([C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)O)[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1>ClCCl>[Cl:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[S:9][C:23]([C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1)([C:31]1[CH:32]=[CH:33][CH:34]=[CH:35][CH:36]=1)[C:25]1[CH:26]=[CH:27][CH:28]=[CH:29][CH:30]=1

참가 물질

5

반응물 3

HCID 6422Trifluoroacetic acidHCID 6457Triphenylcarbinol2회HCID 5194462-Chloro-4-fluorothiophenol

생성물 1

HCID 86684904HCID 86684904, 화합물수율 99.7%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

2-Chloro-4-fluoro-benzenethiol (250 g, 1.54 mol) was dissolved in dichloromethane (1.25 L) and trifluoroacetic acid (120 mL, 1.57 mol) followed by triphenylmethanol (400 g, 1.54 mol) were added at room temperature (ice bath cooling necessary during addition of triphenylmethanol). The mixture was stirred for 1.5 h at room temperature, concentrated and dried in vacuo to yield the title compound as a yellow solid (622 g, 99% purity by HPLC, 99%), that was used without further purification in the next step. 1H NMR (CDCl3, 400 MHz): δ 6.55 (ddd, J=2.9 Hz, 8.0 Hz, 8.9 Hz, 1H), 6.91 (dd, J=6.2 Hz, 8.9 Hz, 1H), 6.97 (dd, J=2.9 Hz, 8.6 Hz, 1H), 7.20-7.27 (m, 9H), 7.34-7.39 (m, 6H).

후처리

  1. additionwere added at room temperature
  2. concentrationconcentrated
  3. customdried in vacuo

출처 및 근거

ORD 기록
ord-bf472721fe7749d7834af2c2649c6ea5
출처 데이터셋
uspto-grants-2014_08
특허 번호
US08796471B2

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