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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Triethylamine → HCID 14347787, 화합물

HRID 2232084
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HRID 2232084 반응식
[CH2:1]([N:8]1[CH2:12][CH:11]([OH:13])[CH:10]([CH2:14]O)[CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(N(CC)CC)C.[CH3:23][S:24](Cl)(=[O:26])=[O:25]>ClCCl>[CH2:1]([N:8]1[CH2:12][CH:11]([OH:13])[CH:10]([CH2:14][S:24]([CH3:23])(=[O:26])=[O:25])[CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 13959884HCID 13959884, 화합물

생성물 1

HCID 14347787HCID 14347787, 화합물수율 93.9%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

1-Benzyl-3-hydroxymethyl-4-hydroxypyrrolidine (66.2 g) and triethylamine (38.8 g) are added to dry dichloromethane (700 ml) and the mixture is cooled till a temperature of from -5° to -10° C. At this temperature, methanesulfonyl chloride (36.6 g) is added dropwise to the mixture with stirring. After the addition, the mixture is stirred for 30 minutes, and then washed with an aqueous sodium hydrogen carbonate and subsequently with water. Thereafter, the dichloromethane layer is separated, dried and concentrated to give 1-benzyl-4-hydroxy-3-methanesulfonylmethylpyrrolidine (80.8 g) as an oil.

후처리

  1. temperaturethe mixture is cooled till a temperature of from -5° to -10° C
  2. additionAfter the addition
  3. stirringthe mixture is stirred for 30 minutes
  4. washwashed with an aqueous sodium hydrogen carbonate and subsequently with water
  5. customThereafter, the dichloromethane layer is separated
  6. customdried
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-f89bde580a284ebcbd0dc7832418e65e
출처 데이터셋
uspto-grants-1988_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04786649

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