Methanesulfonyl chloride → 2,8-Diazaspiro[4.5]decane-2-carboxylic acid, 8-(methylsulfonyl)-, 1,1-dimethylethyl ester

HRID 491475

반응식

HRID 491475 반응식
[C:1]([O:5][C:6]([N:8]1[CH2:12][CH2:11][C:10]2([CH2:17][CH2:16][NH:15][CH2:14][CH2:13]2)[CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].[CH3:18][S:19](Cl)(=[O:21])=[O:20]>C(Cl)Cl.C(N(CC)CC)C>[C:1]([O:5][C:6]([N:8]1[CH2:12][CH2:11][C:10]2([CH2:17][CH2:16][N:15]([S:19]([CH3:18])(=[O:21])=[O:20])[CH2:14][CH2:13]2)[CH2:9]1)=[O:7])([CH3:4])([CH3:2])[CH3:3]

참가 물질

5

반응물 2

HCID 31297Methanesulfonyl chlorideHCID 34178604tert-Butyl 2,8-diazaspiro[4.5]decane-2-carboxylate

생성물 1

HCID 666627142,8-Diazaspiro[4.5]decane-2-carboxylic acid, 8-(methylsulfonyl)-, 1,1-dimethylethyl ester수율 29.6%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 8471Triethylamine용매

실험 절차

To a solution of 2,8-diaza-spiro[4.5]decane-2-carboxylic acid tert-butyl ester (1.12 g, 4.66 mol) in CH2Cl2 (10 ml), triethylamine (3.88 ml) and methanesulfonyl chloride (1.08 ml, 14 mmol) are added at 0° C. The reaction mixture is stirred for overnight, quenched with ice-water and extracted with dichloromethane. The combined extracts are washed with H2O, brine and dried over sodium sulphate to give crude 8-methane sulfonyl-2,8-diaza-spiro[4.5]decane-2-carboxylic acid tert-butyl ester (1.32 g).

후처리

  1. customquenched with ice-water
  2. extractionextracted with dichloromethane
  3. washThe combined extracts are washed with H2O, brine
  4. dry with materialdried over sodium sulphate

출처 및 근거

ORD 기록
ord-4e5c5d59d83841be87b7ac9a8bc2c62b
출처 데이터셋
uspto-grants-2009_05
특허 번호
US07531546B2

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