Butylamine → 6-Chloro-5-amino-4-butyl pyrimidine

HRID 1295465

反応式

HRID 1295465 の反応式
[NH2:1][C:2]1[C:3](Cl)=[N:4][CH:5]=[N:6][C:7]=1[Cl:8].CCN(CC)CC.[CH2:17](N)[CH2:18][CH2:19][CH3:20]>CCCCO>[Cl:8][C:7]1[N:6]=[CH:5][N:4]=[C:3]([CH2:17][CH2:18][CH2:19][CH3:20])[C:2]=1[NH2:1]

参加物

5

反応物 3

HCID 8007ButylamineHCID 8471TriethylamineHCID 794345-Amino-4,6-dichloropyrimidine

生成物 1

HCID 858276526-Chloro-5-amino-4-butyl pyrimidine

試薬・触媒・溶媒 1

HCID 2631-Butanol溶媒

実験手順

A solution of 5-amino-4,6-dichloropyrimidine (1 mmol) in n-BuOH was treated with Et3N (1.2 mmol) and n-Butylamine (1.0 mmol) at 80 C. After 16 h, solvent was removed under reduced pressure. The residue was dissolved in EtOAc, the organic layer washed with water and then dried (MgSO4). Filtration and removal of solvent gave 6-chloro-5-amino-4-butyl pyrimidine as a brown solid. Rf=0.5 in 1:1 EtOAc:hexane. 1H NMR (CDCl3) δ 8.07 (s, 1H), 4.88 (br s, 1H), 3.49 (m, 2H), 3.35 (br s, 2H), 1.6 (m, 2H), 1.44 (m, 2), 0.95 (t, 3H).

後処理

  1. customsolvent was removed under reduced pressure
  2. dissolutionThe residue was dissolved in EtOAc
  3. washthe organic layer washed with water
  4. dry with materialdried (MgSO4)
  5. filtrationFiltration and removal of solvent

出典と根拠

ORDレコード
ord-4c96a5f9caf744acb1e89ce41d429c2c
出典データセット
uspto-grants-2007_07
特許番号
US07241890B2

関連ノート

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