tert-Butyl piperazine-1-carboxylate → 4-(7-Benzyl-3-methyl-2,6-dioxo-2,3,6,7-tetrahydro-1H-purin-8-yl)piperazine-1-carboxylic acid tert-butyl ester

HRID 1792017ノート

反応式

HRID 1792017 の反応式
[CH2:1]([N:8]1[C:16]2[C:15](=[O:17])[NH:14][C:13](=[O:18])[N:12]([CH3:19])[C:11]=2[N:10]=[C:9]1Cl)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:21]([O:25][C:26]([N:28]1[CH2:33][CH2:32][NH:31][CH2:30][CH2:29]1)=[O:27])([CH3:24])([CH3:23])[CH3:22]>C(OCC)(=O)C>[C:21]([O:25][C:26]([N:28]1[CH2:33][CH2:32][N:31]([C:9]2[N:8]([CH2:1][C:2]3[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=3)[C:16]3[C:15](=[O:17])[NH:14][C:13](=[O:18])[N:12]([CH3:19])[C:11]=3[N:10]=2)[CH2:30][CH2:29]1)=[O:27])([CH3:24])([CH3:22])[CH3:23]

参加物

4

反応物 2

HCID 143452tert-Butyl piperazine-1-carboxylateHCID 9115837-benzyl-8-chloro-3-methyl-1H-purine-2,6(3H,7H)-dione

生成物 1

HCID 235369514-(7-Benzyl-3-methyl-2,6-dioxo-2,3,6,7-tetrahydro-1H-purin-8-yl)piperazine-1-carboxylic acid tert-butyl ester収率 96.5%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

7-Benzyl-8-chloro-3-methyl-3,7-dihydropurine-2,6-dione (130 mg) and 1-piperazine carboxylic acid tert-butyl ester (250 mg) were stirred at 150° C. for 1 hour. The reaction mixture was diluted with ethyl acetate, and the resulting suspension was filtered to give white solid. This solid was purified by silica gel column chromatography to obtain 190 mg of the title compound from a fraction eluted with ethyl acetate.

後処理

  1. filtrationthe resulting suspension was filtered
  2. customto give white solid
  3. customThis solid was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-bae984a2d7ad483fb5f6c32628af5994
出典データセット
uspto-grants-2006_07
特許番号
US07074798B2

反応ノート

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