Hydrochloric Acid → 1-Cyclohexyl-4,4-dimethyl-2-(1H-1,2,4-triazol-1-yl)pent-1-en-3-one

HRID 1702162

반응식

HRID 1702162 반응식
[CH3:1][C:2]([CH3:16])([CH3:15])[C:3](=[O:14])[C:4]([N:9]1[CH:13]=[N:12][CH:11]=[N:10]1)=[CH:5]N(C)C.[CH:17]1([Mg]Br)[CH2:22][CH2:21][CH2:20][CH2:19][CH2:18]1.O.Cl>CCOCC>[CH:17]1([CH:5]=[C:4]([N:9]2[CH:13]=[N:12][CH:11]=[N:10]2)[C:3](=[O:14])[C:2]([CH3:1])([CH3:15])[CH3:16])[CH2:22][CH2:21][CH2:20][CH2:19][CH2:18]1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 539360354,4-Dimethyl-1-dimethylamino-2-(1,2,4-triazol-1-yl)-pent-1-en-3-oneHCID 178419651HCID 178419651, 화합물

생성물 1

HCID 566097071-Cyclohexyl-4,4-dimethyl-2-(1H-1,2,4-triazol-1-yl)pent-1-en-3-one수율 83%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

11.1 g (0.05 mol) of 4,4-dimethyl-1-dimethylamino-2-(1,2,4-triazol-1-yl)-pent-1-en-3-one were dissolved in 250 ml of ether. An ethereal solution of 13.1 g (0.07 mol) of cyclohexyl-magnesium bromide was added dropwise to this solution in the course of 30 minutes. The reaction mixture was subsequently stirred for one hour, 250 ml of water were added and the mixture was adjusted to a pH value of 6-7 with hydrochloric acid. The organic phase was separated off, dried and filtered and the filrate was concentrated. 10.8 g (83% of theory) of 1-cyclohexyl-4,4-dimethyl-2-(1,2,4-triazol-1-yl)-pent-1-en-3-one of refractive index nD20 1.5003 were obtained.

후처리

  1. customThe organic phase was separated off
  2. customdried
  3. filtrationfiltered
  4. concentrationthe filrate was concentrated

출처 및 근거

ORD 기록
ord-3c63fa3167c9428c8669cfb4126d2598
출처 데이터셋
uspto-grants-1983_04
특허 번호
US04380628

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