Dichloromethane → HCID 58941891, 화합물

HRID 2097638노트

반응식

HRID 2097638 반응식
[CH:1]([Si:4]([CH:19]([CH3:21])[CH3:20])([CH:16]([CH3:18])[CH3:17])[O:5][CH2:6][C:7]1[S:11][N:10]=[N:9][C:8]=1[C:12]([O:14]C)=O)([CH3:3])[CH3:2].[Cl:22][C:23]1[CH:24]=[C:25]([CH:27]=[CH:28][C:29]=1[F:30])[NH2:26].C(Cl)Cl.C[Al](C)C>CCCCCC>[Cl:22][C:23]1[CH:24]=[C:25]([NH:26][C:12]([C:8]2[N:9]=[N:10][S:11][C:7]=2[CH2:6][O:5][Si:4]([CH:16]([CH3:17])[CH3:18])([CH:19]([CH3:20])[CH3:21])[CH:1]([CH3:2])[CH3:3])=[O:14])[CH:27]=[CH:28][C:29]=1[F:30]

참가 물질

6

반응물 4

HCID 6344DichloromethaneHCID 97083-Chloro-4-fluoroanilineHCID 16682925TrimethylaluminumHCID 58941848HCID 58941848, 화합물

생성물 1

HCID 58941891HCID 58941891, 화합물수율 78.5%

시약·촉매·용매 1

HCID 8058Hexane용매

실험 절차

To a cooled solution (0° C.) of methyl 5-[(triisopropylsilyl)oxy]methyl-1,2,3-thiadiazole-4-carboxylate (2.2 g, 0.0066 mol) and 3-chloro-4-fluoroaniline (1.5 g, 0.010 mol) in DCM (20 mL, 0.4 mol) was added 2.0 M of trimethylaluminum in hexane (12 mL) under nitrogen and stirred for 15 minutes. The volatiles were removed in vacuo and the crude was purified by flash chromatography to give the desired product (2.3 g, 78%). MF═C19H27ClFN3O2SSi; LCMS calculated for C19H28ClFN3O2SSi (M+H)+: m/z=444.1.

후처리

  1. customThe volatiles were removed in vacuo
  2. customthe crude was purified by flash chromatography

출처 및 근거

ORD 기록
ord-1afcc74759c841f5af0dcbbed4e83720
출처 데이터셋
uspto-grants-2013_05
특허 번호
US08450351B2

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