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

HRID 1702162

反応式

HRID 1702162 の反応式
[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

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-3c63fa3167c9428c8669cfb4126d2598
出典データセット
uspto-grants-1983_04
特許番号
US04380628

関連ノート

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