Water → HCID 22004680, 화합물

HRID 369066노트

반응식

HRID 369066 반응식
N1C=CC=CC=1.[NH2:7][CH2:8][CH:9]1[CH2:14][CH2:13][N:12]([C:15]([O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[O:16])[CH2:11][CH2:10]1.[N:22]1[CH:27]=[CH:26][CH:25]=[CH:24][C:23]=1[S:28](Cl)(=[O:30])=[O:29].O>ClCCl>[C:18]([O:17][C:15]([N:12]1[CH2:13][CH2:14][CH:9]([CH2:8][NH:7][S:28]([C:23]2[CH:24]=[CH:25][CH:26]=[CH:27][N:22]=2)(=[O:30])=[O:29])[CH2:10][CH2:11]1)=[O:16])([CH3:21])([CH3:20])[CH3:19]

참가 물질

6

반응물 4

HCID 962WaterHCID 1049PyridineHCID 7368171-Boc-4-(aminomethyl)piperidineHCID 3787675Pyridine-2-sulfonyl Chloride

생성물 1

HCID 22004680HCID 22004680, 화합물수율 47.3%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Pyridine (1.85 ml) was added to a stirred solution of 4-(aminomethyl)-1-(tert-butoxycarbonyl)piperidine (4.46 g) and pyridine-2-sulphonyl chloride (3.7 g) in dichloromethane (110 ml) at -10° C. under a nitrogen atmosphere. The reaction was then warmed to ambient temperature over 16 hours and poured into water (300 ml). The organic layer was separated and further washed with hydrochloric acid (1 M, 2×200 ml), saturated aqueous sodium bicarbonate solution (200 ml) and brine (200 ml). After drying over anhydrous magnesium sulphate, the solution was evaporated to dryness to afford N-{[1-(tert-butoxycarbonyl)-4-piperidyl]methyl}pyridine-2-sulphonamide (3.5 g) as an oil.

후처리

  1. customThe organic layer was separated
  2. washfurther washed with hydrochloric acid (1 M, 2×200 ml), saturated aqueous sodium bicarbonate solution (200 ml) and brine (200 ml)
  3. dry with materialAfter drying over anhydrous magnesium sulphate
  4. customthe solution was evaporated to dryness

출처 및 근거

ORD 기록
ord-0e4a699400ed47f6863108441c9fa01c
출처 데이터셋
uspto-grants-2000_10
특허 번호
US06136825

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