Triethylamine → Tert-butyl 4-(methylsulfonyl)piperidine-1-carboxylate

HRID 390993노트

반응식

HRID 390993 반응식
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][CH:11](O)[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].[CH3:15][S:16](Cl)(=[O:18])=[O:17].C(N(CC)CC)C>ClCCl>[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][CH:11]([S:16]([CH3:15])(=[O:18])=[O:17])[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 643502Tert-butyl 4-hydroxypiperidine-1-carboxylate

생성물 1

HCID 22504298Tert-butyl 4-(methylsulfonyl)piperidine-1-carboxylate

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To 4-hydroxy-piperidine-1-carboxylic acid tert-butyl ester (9.2 g) in dichloromethane (170 ml), stirring at 0° C. was added methanesulfonyl chloride (5.33 ml) and triethylamine (10.24 ml). The reaction mixture was slowly warmed to room temperature and stirred overnight. The reaction mixture was partitioned between chloroform and water. The combined organics were washed with brine and dried (MgSO4). The solvent was removed in vacuo to yield 14 g of 4-methanesulfonyl-piperidine-carboxylic acid tert-butyl ester.

후처리

  1. customThe reaction mixture was partitioned between chloroform and water
  2. washThe combined organics were washed with brine
  3. dry with materialdried (MgSO4)
  4. customThe solvent was removed in vacuo

출처 및 근거

ORD 기록
ord-b2152d600f3f4d5c98ae2cd7583759aa
출처 데이터셋
uspto-grants-2013_02
특허 번호
US08383620B2

반응 노트

불러오는 중…