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Tributylphosphine → HCID 13711424, 화합물

HRID 986413
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HRID 986413 반응식
[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([F:8])[C:3]=1[C:9]1[S:13]S[C:11](=[O:14])[N:10]=1.[Cl:15][C:16]1[C:22]([C:23]([F:26])([F:25])[F:24])=[CH:21][C:20]([Cl:27])=[CH:19][C:17]=1[NH2:18].C(P(CCCC)CCCC)CCC>ClCCl>[Cl:15][C:16]1[C:22]([C:23]([F:25])([F:26])[F:24])=[CH:21][C:20]([Cl:27])=[CH:19][C:17]=1[NH:18][C:11]([NH:10][C:9](=[S:13])[C:3]1[C:2]([F:1])=[CH:7][CH:6]=[CH:5][C:4]=1[F:8])=[O:14]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 13831TributylphosphineHCID 13648922HCID 13648922, 화합물HCID 136718552,5-Dichloro-3-(trifluoromethyl)aniline

생성물 1

HCID 13711424HCID 13711424, 화합물수율 77.8%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

To a solution of 5-(2,6-difluorophenyl)-1,2,4-dithiazole-3-one (0.9 g) in 20 ml of dichloromethane was added dropwise a solution of 2,5-dichloro-3-trifluoromethylaniline (0.9 g) and tributylphosphine (0.8 g) in 10 ml of dichloromethane under ice-cooling and the solution was stirred for 30 minutes at room temperature. The dichloromethane was then distilled off under reduced pressure and to the residue was added ligroin. The precipitated crystal was filtered and the crystal was washed with ligroin to obtain the desired product 1.3 g. (d.p. 176°-177° C.)

후처리

  1. temperaturecooling
  2. distillationThe dichloromethane was then distilled off under reduced pressure and to the residue
  3. additionwas added ligroin
  4. filtrationThe precipitated crystal was filtered
  5. washthe crystal was washed with ligroin

출처 및 근거

ORD 기록
ord-17607399c4f54285805b5f047cb349cb
출처 데이터셋
uspto-grants-1987_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04713396

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