Acetyl chloride → HCID 45082407, 화합물

HRID 62573노트

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HRID 62573 반응식
Cl.[CH3:2][O:3][C:4](=[O:9])[C@@H:5]([CH2:7][OH:8])[NH2:6].C(N(CC)CC)C.[C:17](Cl)(=[O:19])[CH3:18]>ClCCl>[CH3:2][O:3][C:4](=[O:9])[C@@H:5]([CH2:7][OH:8])[NH:6][C:17](=[O:19])[CH3:18]

참가 물질

5

반응물 3

HCID 6367Acetyl chlorideHCID 8471TriethylamineHCID 11446470D-Serine methyl ester hydrochloride

생성물 1

HCID 45082407HCID 45082407, 화합물수율 90%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
-10 °C

실험 절차

D-Serine methyl ester hydrochloride (100 g, 0.6430 mole) was suspended in 500 ml dichloromethane. To this was added triethylamine (136.6 g, 1.35 mole) at 0-5° C., followed by acetyl chloride (53.06 g, 0.6751 mole) drop wise at −10° C. The reaction mixture was stirred at −10° C. for 3 hours, filtered to remove salts and the filtrate was evaporated. The resulting residue was suspended in 400 ml ethyl acetate and stirred for one hour. Salts were filtered and the ethyl acetate layer was concentrated under reduced pressure to get N-acetyl D-serine methyl ester as an oil (93.22 g, Yield: 90%, HPLC: 98.7%),

후처리

  1. filtrationfiltered
  2. customto remove salts
  3. customthe filtrate was evaporated
  4. stirringstirred for one hour
  5. filtrationSalts were filtered
  6. concentrationthe ethyl acetate layer was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-ddb273fd859244429737029322cc5be1
출처 데이터셋
uspto-grants-2016_09
특허 번호
US09447024B1

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