Methyl morpholine oxide → HCID 86658047、化合物

HRID 245355ノート

反応式

HRID 245355 の反応式
[NH2:1][C:2]1[C:6]2[CH:7]=[C:8]([CH2:20][OH:21])[C:9]([N:12]3[CH2:17][C@H:16]([CH3:18])[O:15][C@H:14]([CH3:19])[CH2:13]3)=[C:10]([F:11])[C:5]=2[O:4][N:3]=1.C[N+]1([O-])CCOCC1>C(Cl)Cl.CC#N.CCC[N+](CCC)(CCC)CCC.[O-][Ru](=O)(=O)=O>[NH2:1][C:2]1[C:6]2[CH:7]=[C:8]([CH:20]=[O:21])[C:9]([N:12]3[CH2:17][C@H:16]([CH3:18])[O:15][C@H:14]([CH3:19])[CH2:13]3)=[C:10]([F:11])[C:5]=2[O:4][N:3]=1

参加物

5

反応物 2

HCID 82029Methyl morpholine oxideHCID 67359017{3-amino-6-[(2R,6S)-2,6-dimethylmorpholin-4-yl]-7-fluoro-1,2-benzisoxazol-5-yl}methanol2 回

生成物 1

HCID 86658047HCID 86658047、化合物

試薬・触媒・溶媒 2

HCID 178419074HCID 178419074、化合物触媒HCID 21877088Acetonitrile methylene chloride溶媒

実験手順

To an ice-cooled solution of {3-amino-6-[(2R,6S)-2,6-dimethylmorpholin-4-yl]-7-fluoro-1,2-benzisoxazol-5-yl}methanol (Intermediate 7, 200 mg, 0.67 mmol) in CH2Cl2/CH3CN mixture (4 mL, 1:1 v/v) was added NMO (119 mg, 1.0 mmol) followed TPAP (23 mg, 0.06 mmol) and mixture stirred for 2 h at room temperature. The reaction mixture filtered thorough a silica gel bed and washed with EtOAc. The organic phase concentrated under reduced pressure to give the title compound as a yellow solid. Yield: 100 mg, (50%).

後処理

  1. filtrationThe reaction mixture filtered thorough a silica gel bed
  2. washwashed with EtOAc
  3. concentrationThe organic phase concentrated under reduced pressure

出典と根拠

ORDレコード
ord-5747c39b71a7468ab0b6a51bfede084c
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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