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

HRID 493590

反応式

HRID 493590 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 63651,1-Dichloroethane溶媒

実験手順

A mixture of 4,5-diaminopyrimidine (1.0 g, 9.1 mmol), N-(t-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 3N sodium hydroxide (30 mL). After drying over magnesium sulfate, the organic phase was concentrated to give the title compound as a tan gum. MS 294 (M+1)

後処理

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

出典と根拠

ORDレコード
ord-9e97fb913b8e49cb9bacbe9a0c586c63
出典データセット
uspto-grants-2009_05
特許番号
US07534784B2

関連ノート

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