ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Bromoacetyl bromide → {2-[(2-Bromoacetyl)-(2-methylphenyl)amino]-1,1-dimethylethyl}carbamic acid t-butyl ester

HRID 1694922
ノート
印刷プレビュー

反応式

HRID 1694922 の反応式
[Br:1][CH2:2][C:3](Br)=[O:4].[C:6]([O:10][C:11](=[O:25])[NH:12][C:13]([CH3:24])([CH3:23])[CH2:14][NH:15][C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=1[CH3:22])([CH3:9])([CH3:8])[CH3:7].C(=O)(O)[O-].[Na+]>CN(C)C(=O)C>[C:6]([O:10][C:11](=[O:25])[NH:12][C:13]([CH3:24])([CH3:23])[CH2:14][N:15]([C:3](=[O:4])[CH2:2][Br:1])[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=1[CH3:22])([CH3:9])([CH3:8])[CH3:7]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 61147Bromoacetyl bromideHCID 516892Sodium BicarbonateHCID 66645699[1,1-Dimethyl-2-(2-methylphenylamino)ethyl]carbamic acid t-butyl ester

生成物 1

HCID 66645910{2-[(2-Bromoacetyl)-(2-methylphenyl)amino]-1,1-dimethylethyl}carbamic acid t-butyl ester収率 93.3%

試薬・触媒・溶媒 1

HCID 31374Dimethylacetamide溶媒

実験手順

1.12 ml of bromoacetyl bromide (12.9 mmol) was added to a solution of 2.4 g of [1,1-dimethyl-2-(2-methylphenylamino)ethyl]carbamic acid t-butyl ester obtained in Example (51a) (8.62 mmol) in N,N-dimethylacetamide (85 ml) under ice-cooling, and the mixture was stirred at the same temperature for 10 minutes. A saturated sodium bicarbonate aqueous solution was added to the reaction mixture, followed by extraction with ethyl acetate. Then, the organic layer was washed with water and brine and dried over anhydrous magnesium sulfate. After filtration, the solvent was evaporated under reduced pressure. Hexane was added to the residue, and the solid was collected by filtration to obtain 3.21 g of the title compound (yield: 93%).

後処理

  1. temperaturecooling
  2. extractionfollowed by extraction with ethyl acetate
  3. washThen, the organic layer was washed with water and brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. filtrationAfter filtration
  6. customthe solvent was evaporated under reduced pressure
  7. additionHexane was added to the residue
  8. filtrationthe solid was collected by filtration

出典と根拠

ORDレコード
ord-00c3db40628a43f29a5540398d69111e
出典データセット
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08158790B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート