Triethylamine → HCID 178486032, 화합물

HRID 25594노트

반응식

HRID 25594 반응식
[C:1]([O:5][C:6](=[O:21])[N:7]([C@H:9]1[CH2:14][CH2:13][C@H:12]([CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][OH:20])[CH2:11][CH2:10]1)[CH3:8])([CH3:4])([CH3:3])[CH3:2].[CH3:22][S:23](Cl)(=[O:25])=[O:24].CCN(CC)CC>C(Cl)Cl>[C:1]([O:5][C:6]([N:7]([CH3:8])[C@H:9]1[CH2:10][CH2:11][C@H:12]([CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][O:20][S:23]([CH3:22])(=[O:25])=[O:24])[CH2:13][CH2:14]1)=[O:21])([CH3:3])([CH3:2])[CH3:4]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 178486030HCID 178486030, 화합물

생성물 1

HCID 178486032HCID 178486032, 화합물수율 96.2%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 1.75 g (5.84 mmol) trans-[4-(5-Hydroxy pentyl)-cyclohexyl)-methyl-carbamic acid tert-butyl ester and 0.5 ml (6.42 mmol) of methanesulfonyl chloride in 20 ml CH2Cl2 was added, under cooling with an ice bath, 1.56 ml (11.7 mmol) of Et3N. The mixture was stirred for 3 h at RT. The reaction-mixture was then partitioned between ether/1N HCl and water. The ether-solution was concentrated in vacuo to yield 2.12 g (96%) of clean trans-Methansulfonic acid 5[-4-(tert-butoxy carbonyl-methyl-amino)-cyclohexyl)-pentylester.

후처리

  1. temperatureunder cooling with an ice bath
  2. customThe reaction-mixture was then partitioned between ether/1N HCl and water
  3. concentrationThe ether-solution was concentrated in vacuo

출처 및 근거

ORD 기록
ord-75456389a7a94295bf690ffcd5899ee7
출처 데이터셋
uspto-grants-2005_02
특허 번호
US06858651B2

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