O-Phenylenediamine → 2-[2-amino-phenyl-amino]-6-(3-chloro-phenyl-amino)-9-ethyl-9H-purine

HRID 9907

反応式

HRID 9907 の反応式
Cl[C:2]1[N:10]=[C:9]2[C:5]([N:6]=[CH:7][N:8]2[CH2:11][CH3:12])=[C:4]([NH:13][C:14]2[CH:19]=[CH:18][CH:17]=[C:16]([Cl:20])[CH:15]=2)[N:3]=1.[C:21]1([NH2:28])[CH:26]=[CH:25][CH:24]=[CH:23][C:22]=1[NH2:27]>C(O)CCC>[NH2:27][C:22]1[CH:23]=[CH:24][CH:25]=[CH:26][C:21]=1[NH:28][C:2]1[N:10]=[C:9]2[C:5]([N:6]=[CH:7][N:8]2[CH2:11][CH3:12])=[C:4]([NH:13][C:14]2[CH:19]=[CH:18][CH:17]=[C:16]([Cl:20])[CH:15]=2)[N:3]=1

参加物

4

反応物 2

HCID 7243O-Phenylenediamine2 回HCID 110013202-Chloro-n-(3-chlorophenyl)-9-ethyl-9h-purin-6-amine

生成物 1

HCID 219881902-[2-amino-phenyl-amino]-6-(3-chloro-phenyl-amino)-9-ethyl-9H-purine

試薬・触媒・溶媒 1

HCID 2631-Butanol溶媒

実験手順

Analogously to Example 1, 308 mg (1.0 mmol) of 2-chloro-6-(3-chloro-phenyl-amino)-9-ethyl-9H-purine [described in Stage 1.2] and 324 mg (3 mmol) of 1,2-phenylenediamine are reacted in 10 ml of n-butanol in a glass pressure reactor for 19 h at 140° C., followed by addition of 486 mg (4.5 mmol) of 1,2-phenylenediamine and further reaction at 135° C. for 17 h. After purification by means of column chromatography, 2-[2-amino-phenyl-amino]-6-(3-chloro-phenyl-amino)-9-ethyl-9H-purine is obtained; FAB-MS: (M+H)+=380; HPLC: tret (grad20/2)=11.36 minutes.

後処理

  1. customAfter purification by means of column chromatography

出典と根拠

ORDレコード
ord-bb7bddbd8fa94af28adb4dd86f8741bb
出典データセット
uspto-grants-2006_08
特許番号
US07091346B1

関連ノート

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