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Imidazole → HCID 67462713, 화합물

HRID 1620004
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HRID 1620004 반응식
[OH:1][CH:2]([CH2:20][CH3:21])[C:3]([N:5]1[CH2:10][CH2:9][C:8]2[N:11]=[C:12]([C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=3)[O:13][C:7]=2[CH2:6]1)=[O:4].N1C=CN=C1.[C:27]([Si:31](Cl)([CH3:33])[CH3:32])([CH3:30])([CH3:29])[CH3:28].C(Cl)Cl>CN(C=O)C.CN(C1C=CN=CC=1)C>[C:27]([Si:31]([CH3:33])([CH3:32])[O:1][CH:2]([CH2:20][CH3:21])[C:3]([N:5]1[CH2:10][CH2:9][C:8]2[N:11]=[C:12]([C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=3)[O:13][C:7]=2[CH2:6]1)=[O:4])([CH3:30])([CH3:29])[CH3:28]
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참가 물질

7

반응물 4

HCID 795ImidazoleHCID 6344DichloromethaneHCID 28928tert-Butyldimethylsilyl chlorideHCID 67465313HCID 67465313, 화합물

생성물 1

HCID 67462713HCID 67462713, 화합물

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매
HCID 6228
Dimethylformamide
용매
2회

실험 절차

710.00 mg (2.48 mmol) 2-hydroxy-1-(2-phenyl-6,7-dihydro-4H-oxazolo[5,4-c]pyridin-5-yl)-butan-1-one are placed in 10 mL DMF and combined with 340.00 mg (4.99 mmol) imidazole. Then 600.00 mg (3.98 mmol) tert.-butyl-chloro-dimethyl-silane and 30.00 mg (0.25 mmol) DMAP are added and the mixture is stirred overnight at RT. The DMF is eliminated i.V., the residue is added to DCM and extracted 1 time each with H2O, 1N HCl and saturated sodium chloride solution. The solvent of the org. phase is eliminated in vacuo and the residue is purified on silica gel. (Eluant: cyclohexane/EA).

후처리

  1. extractionextracted 1 time each with H2O, 1N HCl and saturated sodium chloride solution
  2. customthe residue is purified on silica gel

출처 및 근거

ORD 기록
ord-744004ddb0fd49c3938bc89b71a904b1
출처 데이터셋
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08772323B2

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