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Chloroform → N-acetyl-4-hydroxy-L-proline ethyl ester

HRID 1723899
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HRID 1723899 반응식
[C:1](OC(=O)C)(=[O:3])[CH3:2].Cl.[CH2:9]([O:11][C:12](=[O:19])[C@@H:13]1[CH2:17][CH:16]([OH:18])[CH2:15][NH:14]1)[CH3:10].C(N(CC)CC)C.C(Cl)(Cl)Cl>O>[CH2:9]([O:11][C:12](=[O:19])[C@@H:13]1[CH2:17][CH:16]([OH:18])[CH2:15][N:14]1[C:1](=[O:3])[CH3:2])[CH3:10]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 6212ChloroformHCID 7918Acetic AnhydrideHCID 8471TriethylamineHCID 127093054hydroxy-L-proline ethyl ester hydrochloride

생성물 1

HCID 22794895N-acetyl-4-hydroxy-L-proline ethyl ester수율 165.3%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

345 g of acetic anhydride was added dropwise to a suspension of 600 g of 4-hydroxy-L-proline ethyl ester hydrochloride, 683 g of triethylamine and 2.4 L of chloroform at not higher than 10° C. while cooling. After stirring for 2 hours, water (0.6 L) was added, and the layers were separated. The organic layer was dried over magnesium sulfate, and concentrated under reduced pressure to obtain 1020 g of N-acetyl-4-hydroxy-L-proline ethyl ester as an oil.

후처리

  1. temperaturewhile cooling
  2. customthe layers were separated
  3. dry with materialThe organic layer was dried over magnesium sulfate
  4. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-f3f465efaca547fe8bd1b575fb3e8787
출처 데이터셋
uspto-grants-2009_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07485665B2

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