2,2,2-Trifluoroethanol → HCID 117824059、化合物

HRID 59060

反応式

HRID 59060 の反応式
Cl[CH2:2][C:3]1[NH:8][C:7](=[O:9])[NH:6][C:5](=[O:10])[CH:4]=1.[F:11][C:12]([F:16])([F:15])[CH2:13][OH:14].C(=O)([O-])[O-].[Cs+].[Cs+]>CN(C)C=O>[F:11][C:12]([F:16])([F:15])[CH2:13][O:14][CH2:2][C:3]1[NH:8][C:7](=[O:9])[NH:6][C:5](=[O:10])[CH:4]=1

参加物

5

反応物 3

HCID 64092,2,2-TrifluoroethanolHCID 10796Cesium carbonateHCID 732736-(Chloromethyl)-2,4(1H,3H)-pyrimidinedione

生成物 1

HCID 117824059HCID 117824059、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
100 °C

実験手順

A mixture of 6-(chloromethyl)pyrimidine-2,4(1H,3H)-dione (1 g, 6.23 mmol), 2,2,2-trifluoroethanol (2.235 mL, 31.14 mmol) and cesium carbonate (6.09 g, 18.68 mmol) in dimethylformamide (10 mL) was heated in a microwave oven at 100° C. for 30 min. The mixture was filtered and the volatiles were removed in vacuum. The residue was treated with diluted HCl (pH 4.5) and cooled to 0° C. The resulting crystals were collected by filtration and dried in vacuum cabinet to yield the title compound, 0.92 g (66%).

後処理

  1. filtrationThe mixture was filtered
  2. customthe volatiles were removed in vacuum
  3. additionThe residue was treated with diluted HCl (pH 4.5)
  4. temperaturecooled to 0° C
  5. filtrationThe resulting crystals were collected by filtration
  6. customdried in vacuum cabinet

出典と根拠

ORDレコード
ord-f83ca43a663a4b1dbcd984fadc2d0142
出典データセット
uspto-grants-2016_09
特許番号
US09439904B2

関連ノート

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