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Hydrogen Peroxide → HCID 68697894、化合物

HRID 1990892
ノート
印刷プレビュー

反応式

HRID 1990892 の反応式
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][CH:11]([NH:14][C:15]2[O:16][C:17]3[CH:23]=[CH:22][C:21]([C:24]#[N:25])=[CH:20][C:18]=3[N:19]=2)[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].S1C2C=CC=CC=2N=C1NC1CCN(CC2C3C(=CC=CC=3)C=CC=2[O:53]CC)CC1.C(=O)([O-])[O-].[K+].[K+].OO.O>CS(C)=O>[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][CH:11]([NH:14][C:15]2[O:16][C:17]3[CH:23]=[CH:22][C:21]([C:24](=[O:53])[NH2:25])=[CH:20][C:18]=3[N:19]=2)[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:2])[CH3:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 784Hydrogen PeroxideHCID 962WaterHCID 11430Potassium CarbonateHCID 66912254HCID 66912254、化合物HCID 86607625Benzothiazol-2-yl-[1-(2-ethoxy-naphthalen-1-ylmethyl)-piperidin-4-yl]-amine

生成物 1

HCID 68697894HCID 68697894、化合物収率 97%

試薬・触媒・溶媒

1
HCID 679Dimethyl Sulfoxide溶媒

実験手順

To a suspension of 4-(5-cyano-benzooxazol-2-ylamino)-piperidine-1-carboxylic acid tert-butyl ester (1.03 g, 3.01 mmol, 1.0 equiv; intermediate T (2-(piperidin-4-ylamino)-benzooxazole-5-carbonitrile)/step 1) and 0.084 g (0.6 mmol) of potassium carbonate in DMSO (5 mL) was added a solution of 35% hydrogen peroxide in water (0.53 mL, 0.59 g, 6.02 mmol, 2.0 equiv) and the reaction mixture stirred at ambient temperature for 24 h. The solution was poured on crashed ice, the reaction mixture extracted with dichloromethane/2-propanol (4:1, 3×50 mL) and the combined organic phases dried over MgSO4. The organic solvent was evaporated under reduced pressure and the crude reaction product purified with column chromatography on silica eluting with a gradient of dichloromethane/methanol (100:0→95:5) containing 33% of NH4OH to yield 1.05 g (97%) of the title compound. MS (ESI): 361.2 [M+H]+.

後処理

  1. additionThe solution was poured
  2. extractionthe reaction mixture extracted with dichloromethane/2-propanol (4:1, 3×50 mL)
  3. dry with materialthe combined organic phases dried over MgSO4
  4. customThe organic solvent was evaporated under reduced pressure
  5. customthe crude reaction product
  6. custompurified with column chromatography on silica eluting with a gradient of dichloromethane/methanol (100:0→95:5)
  7. additioncontaining 33% of NH4OH

出典と根拠

ORDレコード
ord-fd1bbf8c43ab42ae803c01823de465c6
出典データセット
uspto-grants-2010_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07645753B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート