Water → HCID 86723474、化合物

HRID 2201239ノート

反応式

HRID 2201239 の反応式
[CH3:1][N:2]1[C:7]2=[CH:8][NH:9][C:10]([C:11]3[CH:15]=[CH:14][N:13]([CH3:16])[N:12]=3)=[C:6]2[C:5](=[O:17])[N:4]([CH3:18])[C:3]1=[O:19].Br[CH2:21][CH2:22][CH2:23][C:24]([N:26]([O:28][CH3:29])[CH3:27])=[O:25].C(=O)([O-])[O-].[Cs+].[Cs+].O>CN(C=O)C>[CH3:1][N:2]1[C:7]2=[CH:8][N:9]([CH2:21][CH2:22][CH2:23][C:24]([N:26]([O:28][CH3:29])[CH3:27])=[O:25])[C:10]([C:11]3[CH:15]=[CH:14][N:13]([CH3:16])[N:12]=3)=[C:6]2[C:5](=[O:17])[N:4]([CH3:18])[C:3]1=[O:19]

参加物

6

反応物 4

HCID 962WaterHCID 10796Cesium carbonateHCID 14642623130250-57-62 回HCID 1363484071,3-Dimethyl-5-(1-methyl-1H-pyrazol-3-yl)-1H-pyrrolo[3,4-d]pyrimidine-2,4(3H,6H)-dione

生成物 1

HCID 86723474HCID 86723474、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

1,3-Dimethyl-5-(1-methyl-1H-pyrazol-3-yl)-1H-pyrrolo[3,4-d]pyrimidine-2,4(3H,6H)-dione (800 mg, 3.09 mmol), 4-bromo-N-methoxy-N-methylbutanamide (Intermediate P) (843 mg, 4.01 mmol) and cesium carbonate (2011 mg, 6.17 mmol) were suspended in DMF (11.100 ml) and the mixture was stirred at room temperature for 22 hours. The mixture was poured into water (50 ml) and extracted with DCM (3×100 ml). The combined organic extracts were washed with water (2×50 ml) and brine (50 ml), dried over sodium sulfate and evaporated under vacuum. Purification by mass-directed HPLC under the following conditions afforded the title compound.

後処理

  1. extractionextracted with DCM (3×100 ml)
  2. washThe combined organic extracts were washed with water (2×50 ml) and brine (50 ml)
  3. dry with materialdried over sodium sulfate
  4. customevaporated under vacuum
  5. customPurification by mass-directed HPLC under the following conditions

出典と根拠

ORDレコード
ord-514708b0248943feaf8185d1a94909ed
出典データセット
uspto-grants-2016_06
特許番号
US09359381B2

反応ノート

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