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Acetyl chloride → HCID 86722312、化合物

HRID 874821
ノート
印刷プレビュー

反応式

HRID 874821 の反応式
[O:1]1[CH2:5][CH2:4][O:3][CH:2]1[CH2:6][CH2:7][NH:8][CH2:9][CH2:10][O:11][Si:12]([C:15]([CH3:18])([CH3:17])[CH3:16])([CH3:14])[CH3:13].C(N(C(C)C)CC)(C)C.[C:28](Cl)(=[O:30])[CH3:29]>>[O:1]1[CH2:5][CH2:4][O:3][CH:2]1[CH2:6][CH2:7][N:8]([CH2:9][CH2:10][O:11][Si:12]([C:15]([CH3:18])([CH3:17])[CH3:16])([CH3:14])[CH3:13])[C:28](=[O:30])[CH3:29]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 3

HCID 6367Acetyl chlorideHCID 81531DiisopropylethylamineHCID 86722311HCID 86722311、化合物

生成物 1

HCID 86722312HCID 86722312、化合物収率 65.2%

実験手順

To an ice-cooled solution of N-(2-(1,3-dioxolan-2-yl)ethyl)-2-((tert-butyldimethylsilyl)oxy)ethanamine (0.85 g, 3.09 mmol) and di-iso-propylethylamine (0.82 mL, 4.63 mmol) was added acetyl chloride (0.26 mL, 3.71 mmol). The reaction mixture was stirred with ice-cooling for 1 hour, then the coolant was removed and stirring continued at RT for 18 hours. The reaction mixture was washed with saturated aqueous sodium hydrogen carbonate and the organic phase poured through a hydrophobic frit. The solvent was evaporated at reduced pressure to afford the title compound (0.64 g, 65%).

後処理

  1. temperaturecooling for 1 hour
  2. customthe coolant was removed
  3. stirringstirring
  4. washThe reaction mixture was washed with saturated aqueous sodium hydrogen carbonate
  5. additionthe organic phase poured through a hydrophobic frit
  6. customThe solvent was evaporated at reduced pressure

出典と根拠

ORDレコード
ord-787710981845471baf05038efdd6af29
出典データセット
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08980913B2

反応ノート

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