p-Toluenesulfonic acid → HCID 19012212、化合物

HRID 1646073

反応式

HRID 1646073 の反応式
[Cl:1][C:2]1[N:7]=[C:6]([NH2:8])[C:5]([NH2:9])=[C:4]([CH3:10])[N:3]=1.CO[C:13](OC)(OC)[CH2:14][CH2:15][CH3:16].CC1C=CC(S(O)(=O)=O)=CC=1>COCCO>[Cl:1][C:2]1[N:7]=[C:6]2[C:5]([NH:9][C:13]([CH2:14][CH2:15][CH3:16])=[N:8]2)=[C:4]([CH3:10])[N:3]=1

参加物

5

反応物 3

HCID 6101p-Toluenesulfonic acidHCID 1235121,1,1-TrimethoxybutaneHCID 2752952-Chloro-4,5-diamino-6-methylpyrimidine

生成物 1

HCID 19012212HCID 19012212、化合物収率 47.1%

試薬・触媒・溶媒 1

HCID 80192-Methoxyethanol溶媒

反応条件

温度
140 °C

実験手順

A mixture of 2-Chloro-4,5-diamino-6-methylpyrimidine (0.80 g, 5.04 mmol), trimethylorthobutyrate (1.2 ml, 7.6 mmol) and p-TsOH (0.08 g) in 2-methoxy-ethanol (24 ml) was heated in an oil bath at 140° C. for 24 hours. The product was isolated as described in Step 2 of Example 12 and purified by flash chromatography using EtOAc-hexane (1:1) to give the crystalline titled compound (0.5 g, 47%). NMR(CDCl3): δ1.03 (t, J=8 Hz, 3H), 1.9 (q, 2H), 2.82 (s, 3H), 3.0 (t, J=8 Hz, 2H). FAB-MS: m/e 211 and 213 (M+H). Analysis calculated for C9H11N4Cl: C, 51.31; H, 5.26; N, 26.60. Found: C, 51.43; H, 5.50, N, 26.81.

後処理

  1. customThe product was isolated
  2. custompurified by flash chromatography

出典と根拠

ORDレコード
ord-c39059c1bc3a406ca9cf4fa146b73568
出典データセット
uspto-grants-1993_01
特許番号
US05177074

関連ノート

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