Water → 4,5-Difluoro-6-phenoxypyrimidine

HRID 1871517ノート

反応式

HRID 1871517 の反応式
[C:1]1([OH:7])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.CC(C)([O-])C.[K+].[F:14][C:15]1[C:20]([F:21])=[C:19](F)[N:18]=[CH:17][N:16]=1.O>O1CCCC1>[O:7]([C:19]1[C:20]([F:21])=[C:15]([F:14])[N:16]=[CH:17][N:18]=1)[C:1]1[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

参加物

6

反応物 4

HCID 962WaterHCID 996PhenolHCID 35727644,5,6-TrifluoropyrimidineHCID 23665647Potassium tert-butoxide

生成物 1

HCID 158696744,5-Difluoro-6-phenoxypyrimidine収率 68.1%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
0 °C

実験手順

A solution of 42.4 g (0.45 mol) of phenol and 50.4 g (0.45 mol) of potassium tert-butoxide in 400 ml of tetrahydrofuran is added dropwise at 0° C. to a solution of 80 g (0.6 mol) of 4,5,6-trifluoropyrimidine in 1 l of tetrahydrofuran. When the addition was complete, the reaction mixture was stirred for 30 minutes at 0° C. and then poured into water and extracted using ethyl acetate. The organic phase is dried over sodium sulphate and concentrated in vacuo, and the residue is stirred with low-boiling petroleum ether. 63.8 g (68.1% of theory) of 4-phenoxy-5,6-difluoropyrimidine of melting point 65-66° C. are obtained.

後処理

  1. additionWhen the addition
  2. extractionextracted
  3. dry with materialThe organic phase is dried over sodium sulphate
  4. concentrationconcentrated in vacuo
  5. stirringthe residue is stirred with low-boiling petroleum ether

出典と根拠

ORDレコード
ord-04e217c78e284c6b86f5f1bd59df6a57
出典データセット
uspto-grants-2000_08
特許番号
US06103717

反応ノート

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