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

HRID 1291235
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HRID 1291235 반응식
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
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참가 물질

5

반응물 2

HCID 23694274Sodium methanolate methanolHCID 178430835HCID 178430835, 화합물

생성물 1

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

시약·촉매·용매 2

HCID 935Nickel촉매HCID 887Methanol용매

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온도
50 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-5e9661b82e514bbcbd754ee8b4727446
출처 데이터셋
uspto-grants-1998_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05753664

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