Dichloromethane → HCID 58941891、化合物

HRID 2097638ノート

反応式

HRID 2097638 の反応式
[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]

参加物

6

反応物 4

HCID 6344DichloromethaneHCID 97083-Chloro-4-fluoroanilineHCID 16682925TrimethylaluminumHCID 58941848HCID 58941848、化合物

生成物 1

HCID 58941891HCID 58941891、化合物収率 78.5%

試薬・触媒・溶媒 1

HCID 8058Hexane溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-1afcc74759c841f5af0dcbbed4e83720
出典データセット
uspto-grants-2013_05
特許番号
US08450351B2

反応ノート

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