4,5-Diaminopyrimidine → 4-Amino-5-[(1-t-butoxycarbonylpiperidin-4-yl)amino)pyrimidine

HRID 550369

반응식

HRID 550369 반응식
[NH2:1][C:2]1[C:7]([NH2:8])=[CH:6][N:5]=[CH:4][N:3]=1.[C:9]([O:13][C:14]([N:16]1[CH2:21][CH2:20][C:19](=O)[CH2:18][CH2:17]1)=[O:15])([CH3:12])([CH3:11])[CH3:10].C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+]>ClC(Cl)C>[NH2:1][C:2]1[C:7]([NH:8][CH:19]2[CH2:20][CH2:21][N:16]([C:14]([O:13][C:9]([CH3:12])([CH3:11])[CH3:10])=[O:15])[CH2:17][CH2:18]2)=[CH:6][N:5]=[CH:4][N:3]=1

참가 물질

5

반응물 3

HCID 837034,5-DiaminopyrimidineHCID 735900tert-Butyl 4-oxopiperidine-1-carboxylateHCID 5049666Sodium triacetoxyborohydride

생성물 1

HCID 222932024-Amino-5-[(1-t-butoxycarbonylpiperidin-4-yl)amino)pyrimidine

시약·촉매·용매 1

HCID 63651,1-Dichloroethane용매

실험 절차

A mixture of 4,5-diaminopyrimidine (1.0 g, 9.1 mmol), N-(tert-butoxycarbonyl)-4-piperidone (3.0 g, 15 mmol) and sodium triacetoxyborohydride (1.2 g, 5.6 mmol) in dichloroethane (60 mL) was stirred at room temperature for 3 d. The reaction was partitioned between chloroform (200 mL) and 3 N sodium hydroxide (30 mL). After drying over magnesium sulfate, the organic phase was concentrated to give the title compound as a tan gum. MS: m/z=294 (M+1)

후처리

  1. customThe reaction was partitioned between chloroform (200 mL) and 3 N sodium hydroxide (30 mL)
  2. dry with materialAfter drying over magnesium sulfate
  3. concentrationthe organic phase was concentrated

출처 및 근거

ORD 기록
ord-546aaa8b6b08499385db6e1294eeee5b
출처 데이터셋
uspto-grants-2011_05
특허 번호
US07947678B2

연결된 노트

불러오는 중…