Chlorotrimethylsilane → HCID 178452187、化合物

HRID 884341ノート

反応式

HRID 884341 の反応式
[Zn:1].C[Si](Cl)(C)C.BrCCBr.[C:11]([O:15][C:16]([N:18]1[CH2:21][CH:20]([I:22])[CH2:19]1)=[O:17])([CH3:14])([CH3:13])[CH3:12]>CC(N(C)C)=O>[I-:22].[C:11]([O:15][C:16]([N:18]1[CH2:21][CH:20]([Zn+:1])[CH2:19]1)=[O:17])([CH3:14])([CH3:13])[CH3:12]

参加物

6

反応物 4

HCID 6397ChlorotrimethylsilaneHCID 78391,2-DibromoethaneHCID 23994ZincHCID 11000522Tert-butyl 3-iodoazetidine-1-carboxylate

生成物 1

HCID 178452187HCID 178452187、化合物

試薬・触媒・溶媒 1

HCID 31374Dimethylacetamide溶媒2 回

反応条件

温度
65 °C

実験手順

Zn dust (1.80 g, 27.5 mmol) was vigorously stirred in DMA (11 ml) under nitrogen and the suspension was heated at 65° C. Trimethylsilyl chloride (0.37 g, 3.39 mmol) and 1,2-dibromoethane (0.64 g, 3.39 mmol) was added and stirring continued for 40 min. A solution of 3-iodo-azetidine-1-carboxylic acid tert-butyl ester (6.00 g, 21.2 mmol) in dimethylacetamide (DMA, 10 ml) was then added dropwise to the solution over a period of 30 min and then the reaction mixture allowed to cool to room temperature over 16 h. The resulting solution was used without any purification in the next step.

後処理

  1. temperatureto cool to room temperature over 16 h
  2. customThe resulting solution was used without any purification in the next step

出典と根拠

ORDレコード
ord-6dd1cd814a2a4d8bb3e005b5d492320c
出典データセット
uspto-grants-2012_08
特許番号
US08242102B2

反応ノート

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