Methyl morpholine oxide → HCID 86658113、化合物

HRID 245507ノート

反応式

HRID 245507 の反応式
[F:1][C:2]1[C:11]([CH2:12][OH:13])=[CH:10][C:5]2[C:6]([CH3:9])=[N:7][O:8][C:4]=2[C:3]=1[F:14].C[N+]1([O-])CCOCC1>C(Cl)Cl.CCC[N+](CCC)(CCC)CCC.[O-][Ru](=O)(=O)=O>[F:1][C:2]1[C:11]([CH:12]=[O:13])=[CH:10][C:5]2[C:6]([CH3:9])=[N:7][O:8][C:4]=2[C:3]=1[F:14]

参加物

5

反応物 2

HCID 82029Methyl morpholine oxideHCID 67356869(6,7-Difluoro-3-methyl-1,2-benzisoxazol-5-yl)methanol2 回

生成物 1

HCID 86658113HCID 86658113、化合物

試薬・触媒・溶媒 2

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

実験手順

To an ice-cooled solution of (6,7-difluoro-3-methyl-1,2-benzisoxazol-5-yl)methanol (Intermediate 334, 200 mg, 1.0 mmol) in CH2Cl2 (10 mL) was added NMO (235 mg, 2.0 mmol) followed TPAP (35 mg, 0.1 mmol) and mixture stirred for 2 hours at room temperature. The reaction mixture filtered thorough silica gel bed and washed with EtOAc. The organic phase was concentrated under reduced pressure to give product as a yellow solid. Yield: 150 mg (76%).

後処理

  1. filtrationThe reaction mixture filtered thorough silica gel bed
  2. washwashed with EtOAc
  3. concentrationThe organic phase was concentrated under reduced pressure
  4. customto give product as a yellow solid

出典と根拠

ORDレコード
ord-4da751ce47054cc7819e8d53e8067aa0
出典データセット
uspto-grants-2014_02
特許番号
US08658641B2

反応ノート

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