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Triethylamine → HCID 22253674, 화합물

HRID 1072694
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HRID 1072694 반응식
[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]
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참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 10928Ethyl chloroformateHCID 22253670HCID 22253670, 화합물

생성물 1

HCID 22253674HCID 22253674, 화합물수율 75.2%

시약·촉매·용매 1

HCID 180Acetone용매2회

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-13d0d55dd77045089dbb6100dd87cf67
출처 데이터셋
uspto-grants-2005_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06911510B2

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