Methyl morpholine oxide → HCID 86676738、化合物

HRID 709305ノート

反応式

HRID 709305 の反応式
[OH:1][CH2:2][C:3]1[CH:4]=[C:5]([NH:10][C:11](=[O:30])[C:12]2[CH:17]=[CH:16][C:15]([CH2:18][N:19]3[CH2:24][CH2:23][N:22]([CH3:25])[CH2:21][CH2:20]3)=[C:14]([C:26]([F:29])([F:28])[F:27])[CH:13]=2)[CH:6]=[CH:7][C:8]=1[CH3:9].C[N+]1([O-])CCOCC1>C(Cl)Cl.CCC[N+](CCC)(CCC)CCC.[O-][Ru](=O)(=O)=O>[CH:2]([C:3]1[CH:4]=[C:5]([NH:10][C:11](=[O:30])[C:12]2[CH:17]=[CH:16][C:15]([CH2:18][N:19]3[CH2:20][CH2:21][N:22]([CH3:25])[CH2:23][CH2:24]3)=[C:14]([C:26]([F:29])([F:28])[F:27])[CH:13]=2)[CH:6]=[CH:7][C:8]=1[CH3:9])=[O:1]

参加物

5

反応物 2

HCID 82029Methyl morpholine oxideHCID 67326247HCID 67326247、化合物

生成物 1

HCID 86676738HCID 86676738、化合物収率 88,770.797%

試薬・触媒・溶媒 2

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

実験手順

To a stirred solution of N-(3-(hydroxymethyl)-4-methylphenyl)-4-((4-methylpiperazin-1-yl)methyl)-3-(trifluoromethyl)benzamide (200 mg, 0.47 mmol) in CH2Cl2 (2 mL) was added freshly dried 4 Å MS and NMO (83 mg, 0.71 mmol). The mixture was stirred for 10 min before TPAP (17 mg, 0.05 mmol) was added, and the resulting reaction mixture was stirred 12 hours at room temperature. The reaction mixture was filtered through celite, concentrated under reduced pressure, and purified by flash column chromatography (3% to 7% MeOH/CH2Cl2) to afford title product (175 g, 88% yield). MS m/z: 420 [M+1].

後処理

  1. additionwas added
  2. customthe resulting reaction mixture
  3. filtrationThe reaction mixture was filtered through celite
  4. concentrationconcentrated under reduced pressure
  5. custompurified by flash column chromatography (3% to 7% MeOH/CH2Cl2)

出典と根拠

ORDレコード
ord-4b2b8e63b36e47f9ba4938f8d4d80330
出典データセット
uspto-grants-2015_11
特許番号
US09180127B2

反応ノート

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