Methyl morpholine oxide → HCID 18366609, 화합물

HRID 379591노트

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HRID 379591 반응식
[Br:1][C:2]1[C:10]2[C:9](=[O:11])[N:8]([CH3:12])[C:7](=[O:13])[N:6]([CH2:14][CH:15]([CH3:17])[CH3:16])[C:5]=2[S:4][C:3]=1[CH:18]([OH:29])[C:19]1[N:23]([CH3:24])[C:22]2[CH:25]=[CH:26][CH:27]=[CH:28][C:21]=2[N:20]=1.C[N+]1([O-])CCOCC1>ClCCl.[Ru]([O-])(=O)(=O)=O.C([N+](CCC)(CCC)CCC)CC>[Br:1][C:2]1[C:10]2[C:9](=[O:11])[N:8]([CH3:12])[C:7](=[O:13])[N:6]([CH2:14][CH:15]([CH3:17])[CH3:16])[C:5]=2[S:4][C:3]=1[C:18]([C:19]1[N:23]([CH3:24])[C:22]2[CH:25]=[CH:26][CH:27]=[CH:28][C:21]=2[N:20]=1)=[O:29]

참가 물질

5

반응물 2

HCID 82029Methyl morpholine oxideHCID 18366606HCID 18366606, 화합물

생성물 1

HCID 18366609HCID 18366609, 화합물수율 58.8%

시약·촉매·용매 2

HCID 178419074HCID 178419074, 화합물촉매HCID 6344Dichloromethane용매

실험 절차

Prepared according to the method described in Example 37 step c from 5-bromo-6-[hydroxy(1-methyl-1H-benzimidazol-2-yl)methyl]-3-methyl-1-(2-methylpropyl)-thieno[2,3-d]pyrimidine-2,4(1H,3H)-dione (5.0 g), 4-methylmorpholine-N-oxide (1.84 g), powdered 4 Å sieves (5.0 g) and tetra-n-propyl-ammonium perruthenate (0.18 g) in dry dichloromethane (170 ml) with stirring at room temperature for 24 hours. After work up, the residue was purified by column chromatography over silica eluting with a gradient of 0-2% ethanol in dichloromethane to give the subtitle compound as a yellow powder (2.93 g).

후처리

  1. customPrepared
  2. customAfter work up, the residue was purified by column chromatography over silica eluting with a gradient of 0-2% ethanol in dichloromethane

출처 및 근거

ORD 기록
ord-da46f104d2564f07980f85e01e57ed5c
출처 데이터셋
uspto-grants-2001_10
특허 번호
US06300334B1

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