3-Amino-1-propanol → 3-[(2-Chloro-5-methyl-4-pyrimidinyl)amino]-1-propanol

HRID 603482ノート

反応式

HRID 603482 の反応式
[Cl:1][C:2]1[N:7]=[C:6](Cl)[C:5]([CH3:9])=[CH:4][N:3]=1.[NH2:10][CH2:11][CH2:12][CH2:13][OH:14].C(=O)([O-])[O-].[Na+].[Na+]>C(O)C>[Cl:1][C:2]1[N:7]=[C:6]([NH:10][CH2:11][CH2:12][CH2:13][OH:14])[C:5]([CH3:9])=[CH:4][N:3]=1

参加物

5

反応物 3

HCID 90863-Amino-1-propanolHCID 10340Sodium CarbonateHCID 74508Pyrimidine, 2,4-dichloro-5-methyl-

生成物 1

HCID 593004463-[(2-Chloro-5-methyl-4-pyrimidinyl)amino]-1-propanol収率 99%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a solution of 2,4-dichloro-5-methylpyrimidine (8.00 g, 49.1 mmol) and 3-amino-1-propanol (4.50 mL, 58.9 mmol) in ethanol (200 mL) was added sodium carbonate (26.0 g, 245 mmol). The solution was vigorously stirred at rt for 24 h. The mixture was filtered over Celite® and the filtrate concentrated under reduced pressure. The resulting solid was triturated with Et2O to give the product as a white solid (9.80 g, 99%). 1H NMR (400 MHz, CDCl3) δ 1.86 (qt, 2H), 2.00 (s, 3H), 3.55 (t, 2H), 3.64 (t, 2H), 4.92 (broad, 2H), 7.68 (s, 1H).

後処理

  1. filtrationThe mixture was filtered over Celite®
  2. concentrationthe filtrate concentrated under reduced pressure
  3. customThe resulting solid was triturated with Et2O

出典と根拠

ORDレコード
ord-7482790f3bd74f7bae846a757584515a
出典データセット
uspto-grants-2011_03
特許番号
US07906653B2

反応ノート

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