Triphenylphosphine → 1-Benzyloxy-3,5-dichloro-4-(3-(4-trifluoromethylbenzamido)propyloxy)benzene

HRID 323682

반응식

HRID 323682 반응식
[F:1][C:2]([F:17])([F:16])[C:3]1[CH:15]=[CH:14][C:6]([C:7]([NH:9][CH2:10][CH2:11][CH2:12][OH:13])=[O:8])=[CH:5][CH:4]=1.[CH2:18]([O:25][C:26]1[CH:31]=[C:30]([Cl:32])[C:29](O)=[C:28]([Cl:34])[CH:27]=1)[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.N(C(OC(C)C)=O)=NC(OC(C)C)=O>O1CCCC1>[CH2:18]([O:25][C:26]1[CH:27]=[C:28]([Cl:34])[C:29]([O:13][CH2:12][CH2:11][CH2:10][NH:9][C:7](=[O:8])[C:6]2[CH:14]=[CH:15][C:3]([C:2]([F:16])([F:17])[F:1])=[CH:4][CH:5]=2)=[C:30]([Cl:32])[CH:31]=1)[C:19]1[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=1

참가 물질

6

반응물 4

HCID 11776TriphenylphosphineHCID 75555Diisopropyl diazene-1,2-dicarboxylateHCID 120841702,6-Dichloro-4-benzyloxyphenolHCID 220068303-(4-Trifluoromethylbenzamido)propan-1-ol

생성물 1

HCID 220068441-Benzyloxy-3,5-dichloro-4-(3-(4-trifluoromethylbenzamido)propyloxy)benzene

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

A reaction vessel was charged with 5.25 g (21.2 mmol) of 3-(4-(trifluoromethyl)benzamido)propan-1-ol, 5.72 g (21.2 mmol) of 4-benzyloxy-2,6-dichlorophenol, 5.29 g (20.2 mmol) of triphenylphosphine and 100 ml of tetrahydrofuran, and a solution of 4.08 g (20.2 mmol) of diisopropyl azodicarboxylate dissolved in 20 ml of tetrahydrofuran was added dropwise, while stirring. After stirring at room temperature for 12 hours, the reaction mixture was concentrated, and the residue was subjected to silica gel chromatography, which afforded 1-benzyloxy-3,5-dichloro-4-(3-(4-trifluoromethylbenzamido)propyloxy)benzene.

후처리

  1. additionwas added dropwise
  2. stirringAfter stirring at room temperature for 12 hours
  3. concentrationthe reaction mixture was concentrated

출처 및 근거

ORD 기록
ord-a235087b54ae433b85bd26c2d88c5080
출처 데이터셋
uspto-grants-2001_04
특허 번호
US06214835B1

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