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Hydrochloric Acid → HCID 54324090, 화합물

HRID 568312
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HRID 568312 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][C:9]([CH3:23])([CH3:22])[C:10](=[O:21])[C:11]([N:16]2[CH:20]=[N:19][CH:18]=[N:17]2)=[CH:12]N(C)C)=[CH:4][CH:3]=1.[CH2:24]([Mg]Br)[CH2:25][CH3:26].Cl>CCOCC>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([CH2:8][C:9]([CH3:22])([CH3:23])[C:10](=[O:21])[C:11]([N:16]2[CH:20]=[N:19][CH:18]=[N:17]2)=[CH:12][CH2:24][CH2:25][CH3:26])=[CH:6][CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 53860039HCID 53860039, 화합물HCID 178455851HCID 178455851, 화합물

생성물 1

HCID 54324090HCID 54324090, 화합물수율 60.5%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

49.9 g (0.15 mol) of 1-(4-chlorophenyl)-2,2-dimethyl-5-dimethylamino-4-(1,2,4-triazol-1-yl)-4-penten-3-one are dissolved in 750 ml of ether, and a solution of 33.9 g (0.23 mol) of n-propyl-magnesium bromide in 100 ml of ether is added dropwise at -20° C. The reaction mixture is subsequently stirred for 1.5 hours, during which it warms to room temperature. The reaction mixture is adjusted to a pH value of 7 to 8 with dilute hydrochloric acid. The organic phase is then separated off, washed with water, dried over sodium sulphate and concentrated. The residue is purified by column chromatography (silica gel; ethyl acetate/cyclohexane=3:1). 30.1 g (60.5% of theory) of 1-(4-chlorophenyl)-2,2-dimethyl-4-(1,2,4-triazol-1-yl)-4-octen-3-one of refractive index nD20 1.5429 are obtained.

후처리

  1. customwarms to room temperature
  2. customThe organic phase is then separated off
  3. washwashed with water
  4. dry with materialdried over sodium sulphate
  5. concentrationconcentrated
  6. customThe residue is purified by column chromatography (silica gel; ethyl acetate/cyclohexane=3:1)

출처 및 근거

ORD 기록
ord-5c86b09bac89485f8e704dd8fbbf0861
출처 데이터셋
uspto-grants-1988_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04728356

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