Methyl morpholine oxide → HCID 18366609、化合物

HRID 379591ノート

反応式

HRID 379591 の反応式
[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]

参加物

5

反応物 2

HCID 82029Methyl morpholine oxideHCID 18366606HCID 18366606、化合物

生成物 1

HCID 18366609HCID 18366609、化合物収率 58.8%

試薬・触媒・溶媒 2

HCID 178419074HCID 178419074、化合物触媒HCID 6344Dichloromethane溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-da46f104d2564f07980f85e01e57ed5c
出典データセット
uspto-grants-2001_10
特許番号
US06300334B1

反応ノート

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