Sodium methanolate methanol → 7-Deazahypoxanthine

HRID 1291234

反応式

HRID 1291234 の反応式
S[C:2]1[NH:3][C:4](=[O:11])[C:5]2[CH:10]=[CH:9][NH:8][C:6]=2[N:7]=1.C[O-].[Na+].CO>CO.[Ni]>[N:7]1[C:6]2[NH:8][CH:9]=[CH:10][C:5]=2[C:4](=[O:11])[NH:3][CH:2]=1

参加物

5

反応物 2

HCID 23694274Sodium methanolate methanolHCID 178518762HCID 178518762、化合物

生成物 1

HCID 1354086897-Deazahypoxanthine収率 66.5%

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 887Methanol溶媒

反応条件

温度
50 °C

実験手順

In methanol (714 ml) was suspended 2-mercapto-7H-pyrrolo[2,3-d]pyrimidin-4(3H)-one (15.06 g) followed by addition of 28% sodium methoxide/methanol (18.4 ml). While this solution was stirred at 50° C., Raney nickel was added until disappearance of the starting compound had been verified by TLC. The catalyst was then filtered off and the filtrate was neutralized with 1N-HCl (90 ml). The solvent was then distilled off under reduced pressure and the resulting precipitate was collected by filtration, rinsed serially with water, methanol and ether, and dried to provide the title compound (8.1 g). 1H-NMR (DMSO-d6) 8: 6.44(1H,d,J=3.0Hz), 7.03(1H,d,J=3.OHz), 7.83(1H,s), 11.80(1H,brs).

後処理

  1. filtrationThe catalyst was then filtered off
  2. distillationThe solvent was then distilled off under reduced pressure
  3. filtrationthe resulting precipitate was collected by filtration
  4. washrinsed serially with water, methanol and ether
  5. customdried

出典と根拠

ORDレコード
ord-518e9f0b1ad34c5aa6dfe261ee7b5f7e
出典データセット
uspto-grants-1998_05
特許番号
US05753664

関連ノート

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