t-Butyl 4-Fluoroacetoacetate → HCID 178516166、化合物

HRID 1111270

反応式

HRID 1111270 の反応式
[F:1][CH2:2][C:3](=O)[CH2:4][C:5]([O:7]C(C)(C)C)=O.[NH2:13][C:14]1[N:18]=[C:17]([S:19][CH2:20][C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)[NH:16][N:15]=1>C(O)(=O)C>[CH2:20]([S:19][C:17]1[N:18]=[C:14]2[N:13]=[C:3]([CH2:2][F:1])[CH:4]=[C:5]([OH:7])[N:15]2[N:16]=1)[C:21]1[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=1

参加物

4

反応物 2

HCID 15029427t-Butyl 4-FluoroacetoacetateHCID 178509291HCID 178509291、化合物

生成物 1

HCID 178516166HCID 178516166、化合物

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

A solution containing 20.0 g (114 mmol) of t-butyl 4-fluoroacetoacetate, 23.4 g (114 mmol) of 3-amino-5-benzylthio-1,2,4-triazole in 250 ml of glacial acetic acid was heated at reflux with stirring for 5.5 hr and then allowed to cool and stand overnight. The crystals that formed were ground to reduce their size and then recovered by filtration and dried in a vacuum oven to obtain 18.3 g (55 percent of theory) of the title product as a white powder melting with decomposition at 214°-218° C.

後処理

  1. temperaturewas heated
  2. temperatureat reflux
  3. temperatureto cool
  4. waitstand overnight
  5. customThe crystals that formed
  6. filtrationrecovered by filtration
  7. customdried in a vacuum oven

出典と根拠

ORDレコード
ord-5ee8dab487404f6e8e34b3a1d2f23b71
出典データセット
uspto-grants-1990_12
特許番号
US04979981

関連ノート

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