Water → HCID 57973805、化合物

HRID 1863926ノート

反応式

HRID 1863926 の反応式
[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

参加物

6

反応物 4

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

生成物 1

HCID 57973805HCID 57973805、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-a0243bf99bc442e2a0f82c954d4edfea
出典データセット
uspto-grants-2009_12
特許番号
US07625888B2

反応ノート

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