Allylamine → 2-Allylamino-7-methyl-4-neopentylaminothieno[3,2-d] pyrimidine

HRID 1250621ノート

反応式

HRID 1250621 の反応式
[CH2:1]([NH2:4])[CH:2]=[CH2:3].Cl[C:6]1[N:7]=[C:8]([NH:16][CH2:17][C:18]([CH3:21])([CH3:20])[CH3:19])[C:9]2[S:14][CH:13]=[C:12]([CH3:15])[C:10]=2[N:11]=1>O>[CH2:1]([NH:4][C:6]1[N:7]=[C:8]([NH:16][CH2:17][C:18]([CH3:21])([CH3:20])[CH3:19])[C:9]2[S:14][CH:13]=[C:12]([CH3:15])[C:10]=2[N:11]=1)[CH:2]=[CH2:3]

参加物

4

反応物 2

HCID 7853AllylamineHCID 183264882-Chloro-7-methyl-4-neopentylaminothieno[3,2-d]pyrimidine

生成物 1

HCID 207187172-Allylamino-7-methyl-4-neopentylaminothieno[3,2-d] pyrimidine収率 63.1%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
140 °C

実験手順

In 2.28 g (40.0 mmol) of allylamine was dissolved 250 mg (0.9 mmol) of 2-chloro-7-methyl-4-neopentylaminothieno[3,2-d]pyrimidine, and the resulting solution was heated in a sealed tube at 140° C. for 24 hours. After the reaction mixture was cooled, 100 ml of water was added thereto, followed by extraction with ethyl acetate (20 ml×3). The organic layer was washed with 20 ml of water and dried over anhydrous sodium sulfate, and then the solvent was distilled off. The residue was purified by silica gel column chromatography (eluent: ethyl acetate-hexane=1/4) to give 165 mg (yield: 61.3%) of the title compound.

後処理

  1. temperatureAfter the reaction mixture was cooled
  2. extractionfollowed by extraction with ethyl acetate (20 ml×3)
  3. washThe organic layer was washed with 20 ml of water
  4. dry with materialdried over anhydrous sodium sulfate
  5. distillationthe solvent was distilled off
  6. customThe residue was purified by silica gel column chromatography (eluent: ethyl acetate-hexane=1/4)

出典と根拠

ORDレコード
ord-f7636c58f46944e68fb38628c3653a80
出典データセット
uspto-grants-2002_01
特許番号
US06339089B2

反応ノート

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