t-Butyl 4-Fluoroacetoacetate → HCID 178516166, 화합물

HRID 1111270

반응식

HRID 1111270 반응식
[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

참가 물질

4

반응물 2

HCID 15029427t-Butyl 4-FluoroacetoacetateHCID 178509291HCID 178509291, 화합물

생성물 1

HCID 178516166HCID 178516166, 화합물

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-5ee8dab487404f6e8e34b3a1d2f23b71
출처 데이터셋
uspto-grants-1990_12
특허 번호
US04979981

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