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Acetonitrile → HCID 12899882, 화합물

HRID 2198766
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HRID 2198766 반응식
[F:1][CH2:2][C:3]([CH2:17][F:18])([CH3:16])[C:4](=[O:15])[CH:5](Br)[O:6][C:7]1[CH:12]=[CH:11][C:10]([Cl:13])=[CH:9][CH:8]=1.N1C=[CH:22][N:21]=[N:20]1.[C:24](#[N:26])C>>[F:1][CH2:2][C:3]([CH2:17][F:18])([CH3:16])[C:4](=[O:15])[CH:5]([O:6][C:7]1[CH:12]=[CH:11][C:10]([Cl:13])=[CH:9][CH:8]=1)[N:21]1[CH:22]=[N:26][CH:24]=[N:20]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 6342AcetonitrileHCID 130194363,3-Bis-fluoromethyl-1-bromo-1-(4-chlorophenoxy)-butan-2-oneHCID 178418936HCID 178418936, 화합물

생성물 1

HCID 12899882HCID 12899882, 화합물수율 71%

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온도
50 °C

실험 절차

190 g (0.557 mol) of 3,3-bisfluoromethyl-1-bromo-1-(4-chlorophenoxy)-butan-2-one and 90 g (1.3 mols) of triazole were introduced into 800 ml of acetonitrile, the mixture was heated at 50° C. for 5 hours, the solvent was distilled off under a waterpump vacuum, the residue was taken up in one liter of methylene chloride and washed twice with 1,000 ml of water each time, the organic phase was dried over sodium sulphate and the solvent was distilled off. The residue was taken up in 500 ml of diisopropyl ether and the precipitate was filtered off. The mother liquor was distilled. 130.5 g (71% of theory) of 3,3-bisfluoromethyl-1-(4-chlorophenoxy)-1-(1,2,4-triazol-1-yl)-butan-2-one of boiling point 160°-66° C./0.2 mm Hg were obtained. ##STR76##

후처리

  1. distillationthe solvent was distilled off under a waterpump vacuum
  2. washwashed twice with 1,000 ml of water each time
  3. dry with materialthe organic phase was dried over sodium sulphate
  4. distillationthe solvent was distilled off
  5. filtrationthe precipitate was filtered off
  6. distillationThe mother liquor was distilled

출처 및 근거

ORD 기록
ord-5ded20473a3d43a1b42bed03d4f8c101
출처 데이터셋
uspto-grants-1982_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04359470

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