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Lawesson's reagent → HCID 22346994, 화합물

HRID 897877
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인쇄 미리보기

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HRID 897877 반응식
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9](=O)[C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=2[F:16])=[CH:4][CH:3]=1.COC1C=CC(P2(=S)SP(=S)(C3C=CC(OC)=CC=3)[S:27]2)=CC=1>C1(C)C=CC=CC=1>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=2[F:16])=[S:27])=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 87949Lawesson's reagentHCID 531936HCID 531936, 화합물

생성물 1

HCID 22346994HCID 22346994, 화합물수율 178.3%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

A mixture of N1-(4-bromophenyl)-2-fluorobenzamide (3.3 g, 0.0112 mol) and 2,4-bis-(4-methoxyphenyl)-1,3-dithia-2,4-diphosphetane-2,4-disulfide (2.27 g, 0.00561 mol) was heated in toluene at reflux under an atmosphere of nitrogen for 3 hours. The reaction mixture was cooled to ambient temperature, the solvent was removed under reduced pressure and the residue was purified by flash chromatography on silica using ethyl acetate/n-heptane (1:6) as mobile phase to yield N1-(4-bromophenyl)-2-fluoro-1-benzenecarbothioamide (3.1 g, 0.010 mol) as a yellow solid.

후처리

  1. temperatureat reflux under an atmosphere of nitrogen for 3 hours
  2. customthe solvent was removed under reduced pressure
  3. customthe residue was purified by flash chromatography on silica

출처 및 근거

ORD 기록
ord-e632914176994e0e977e0c97a15fe7f0
출처 데이터셋
uspto-grants-2005_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06921763B2

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