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Triethylamine → HCID 22253674、化合物

HRID 226196
ノート
印刷プレビュー

反応式

HRID 226196 の反応式
[Br:1][CH:2]([CH3:12])[C:3]([NH:5][C:6]([CH3:11])([CH3:10])[C:7]([OH:9])=[O:8])=O.C(N(CC)CC)C.ClC(OCC)=O>CC(C)=O>[Br:1][CH:2]([C:3]1[O:8][C:7](=[O:9])[C:6]([CH3:11])([CH3:10])[N:5]=1)[CH3:12]
参加物反応条件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 8471TriethylamineHCID 10928Ethyl chloroformateHCID 22253670HCID 22253670、化合物

生成物 1

HCID 22253674HCID 22253674、化合物

試薬・触媒・溶媒 1

HCID 180Acetone溶媒2 回

反応条件

温度
5 °C

実験手順

To a stirring mixture of 2-(2-bromopropionylamino)-2-methyl propionic acid (50.00 g, 0.21 mol), triethylamine (23.37 g, 0.23 mol), and 150 mL acetone cooled to 5° C., was added dropwise a solution of ethyl chloroformate (25.07 g, 0.23 mol) in 40 mL acetone. After full addition, the mixture was allowed to warm to room temperature, and was stirred for two hours. The mixture was filtered, and the solid was washed with ether. The solvent was then removed under vacuum, and the residue was filtered. The filtrate was distilled under reduced pressure to give a colorless oil (bp 63-64° C. at 1 mmHg). A yield of 34.73 g (75%) was obtained.

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート

後処理

  1. additionAfter full addition
  2. temperatureto warm to room temperature
  3. filtrationThe mixture was filtered
  4. washthe solid was washed with ether
  5. customThe solvent was then removed under vacuum
  6. filtrationthe residue was filtered
  7. distillationThe filtrate was distilled under reduced pressure
  8. customto give a colorless oil (bp 63-64° C. at 1 mmHg)
  9. customA yield of 34.73 g (75%) was obtained

出典と根拠

ORDレコード
ord-f1583da24e854b89b45dd0f389a50517
出典データセット
uspto-grants-2009_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07557177B2

反応ノート

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