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Sodium methanolate methanol → 5-methyl-3H-pyrrolo[2,3-d]pyrimidin-4(7H)-one

HRID 1291235
ノート
印刷プレビュー

反応式

HRID 1291235 の反応式
S[C:2]1[NH:3][C:4](=[O:12])[C:5]2[C:10]([CH3:11])=[CH:9][NH:8][C:6]=2[N:7]=1.C[O-].[Na+].CO>CO.[Ni]>[CH3:11][C:10]1[C:5]2[C:4](=[O:12])[NH:3][CH:2]=[N:7][C:6]=2[NH:8][CH:9]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 23694274Sodium methanolate methanolHCID 178430835HCID 178430835、化合物

生成物 1

HCID 1357418185-methyl-3H-pyrrolo[2,3-d]pyrimidin-4(7H)-one収率 65.3%

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-5-methyl-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 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) δ: 6.44(1H,d,J=3.OHz), 7.03(1H,d,J=3.0 Hz), 7.83(1H,s), 11.80(1H,brs).

後処理

  1. filtrationThe catalyst was then filtered off
  2. distillationThe solvent was 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-5e9661b82e514bbcbd754ee8b4727446
出典データセット
uspto-grants-1998_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05753664

反応ノート

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