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Triethylamine → HCID 22253674、化合物

HRID 353503
ノート
印刷プレビュー

反応式

HRID 353503 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、化合物収率 75.2%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒2 回

実験手順

To a stirring mixture of 2-(2-bromo-propionylamino)-2-methyl-propionic acid (50.0 g; 0.21 mol), triethylamine (23.37 g; 0.23 mol) and 150 mL acetone, cooled with an ice bath, was added a solution of ethyl chloroformate (25.07 g; 0.23 mol) in 40 mL acetone over a period of 10 minutes. The reaction mixture was then allowed to warm to room temperature and was stirred for 2 hours. The mixture was then filtered, and the solid was washed with 150 mL ether. The combined filtrate was concentrated under vacuum. Ether (100 mL) was added to the residue, and the mixture was filtered. After removal of the solvent under vacuum, the filtrate residue was distilled under reduced pressure (63-64° C.; 1 mmHg) to give 34.73 g (75%) of a colorless oil.

後処理

  1. temperaturecooled with an ice bath
  2. filtrationThe mixture was then filtered
  3. washthe solid was washed with 150 mL ether
  4. concentrationThe combined filtrate was concentrated under vacuum
  5. additionEther (100 mL) was added to the residue
  6. filtrationthe mixture was filtered
  7. customAfter removal of the solvent under vacuum
  8. distillationthe filtrate residue was distilled under reduced pressure (63-64° C.; 1 mmHg)

出典と根拠

ORDレコード
ord-28ef0a4faf8c426b9f68996cb26bc645
出典データセット
uspto-grants-2004_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06753391B1

反応ノート

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