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Hydrogen Peroxide → HCID 68697894, 화합물

HRID 1990892
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HRID 1990892 반응식
[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]
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참가 물질

7

반응물 5

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

생성물 1

HCID 68697894HCID 68697894, 화합물수율 97%

시약·촉매·용매

1
HCID 679Dimethyl Sulfoxide용매

실험 절차

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]+.

후처리

  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

출처 및 근거

ORD 기록
ord-fd1bbf8c43ab42ae803c01823de465c6
출처 데이터셋
uspto-grants-2010_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07645753B2

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