Water → HCID 57973805, 화합물

HRID 1863926노트

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HRID 1863926 반응식
[F:1][C:2]([F:15])([F:14])[C:3]1[N:4]=[CH:5][C:6]2[CH2:12][CH2:11][NH:10][C:9](=[O:13])[C:7]=2[N:8]=1.[C:16](=O)([O-])[O-].[Na+].[Na+].F[B-](F)(F)F.C[O+](C)C.O>ClCCl>[CH3:16][O:13][C:9]1[C:7]2[N:8]=[C:3]([C:2]([F:1])([F:14])[F:15])[N:4]=[CH:5][C:6]=2[CH2:12][CH2:11][N:10]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 10340Sodium CarbonateHCID 2735153Oxonium, trimethyl-, tetrafluoroborate(1-) (1:1)HCID 68523413HCID 68523413, 화합물

생성물 1

HCID 57973805HCID 57973805, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a vigorously stirred mixture of 336 mg (1.33 mmol) of 2-(trifluoromethyl)-6,7-dihydropyrido[3,4-d]pyrimidin-8(5H)-one and 2.94 g (27.7 mmol) of anhydrous sodium carbonate in 15 mL of dichloromethane was added 979 mg (6.6 mmol) of trimethyloxonium tetrafluoroborate. Vigorous stirring was continued at room temperature for 5.5 h. Then 15 mL of water was added, and the mixture was shaken. After separation of the phases, the aqueous layer was extracted twice with dichloromethane. The combined organic fractions were dried over sodium sulfate, filtered, and concentrated. Purification of the residue by flash chromatography on silica gel (0-2% methanol in dichloromethane) yielded the title compound as a yellow solid. LC-MS 232 (M+1).

후처리

  1. stirringthe mixture was shaken
  2. customAfter separation of the phases
  3. extractionthe aqueous layer was extracted twice with dichloromethane
  4. dry with materialThe combined organic fractions were dried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customPurification of the residue by flash chromatography on silica gel (0-2% methanol in dichloromethane)

출처 및 근거

ORD 기록
ord-a0243bf99bc442e2a0f82c954d4edfea
출처 데이터셋
uspto-grants-2009_12
특허 번호
US07625888B2

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