Sodium methanolate methanol → 7-Deazahypoxanthine

HRID 1291234

반응식

HRID 1291234 반응식
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

참가 물질

5

반응물 2

HCID 23694274Sodium methanolate methanolHCID 178518762HCID 178518762, 화합물

생성물 1

HCID 1354086897-Deazahypoxanthine수율 66.5%

시약·촉매·용매 2

HCID 935Nickel촉매HCID 887Methanol용매

반응 조건

온도
50 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-518e9f0b1ad34c5aa6dfe261ee7b5f7e
출처 데이터셋
uspto-grants-1998_05
특허 번호
US05753664

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