Water → 1,1-Dichloro-3-(4-chlorophenyl)-3-hydroxy-4-(1,2,4-(1H)-triazolyl)but-1-ene

HRID 1651085ノート

反応式

HRID 1651085 の反応式
[Cl:1][CH:2]([Cl:19])[CH2:3][C:4]([C:12]1[CH:17]=[CH:16][C:15]([Cl:18])=[CH:14][CH:13]=1)([OH:11])[CH2:5][N:6]1[CH:10]=[N:9][CH:8]=[N:7]1.N1C=N[C-]=N1.[Na+].O.C(OCC)C>CN(C)C=O>[Cl:19][C:2]([Cl:1])=[CH:3][C:4]([C:12]1[CH:17]=[CH:16][C:15]([Cl:18])=[CH:14][CH:13]=1)([OH:11])[CH2:5][N:6]1[CH:10]=[N:9][CH:8]=[N:7]1

参加物

6

反応物 4

HCID 962WaterHCID 3283Diethyl EtherHCID 150864851,1-dichloro-3-(4-chlorophenyl)-3-hydroxy-4-(1,2,4-(1H)-triazolyl)butaneHCID 547199651,2,4-Triazolylsodium

生成物 1

HCID 150864861,1-Dichloro-3-(4-chlorophenyl)-3-hydroxy-4-(1,2,4-(1H)-triazolyl)but-1-ene

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A solution of 5.0 g (0.014 mol) of 1,1-dichloro-3-(4-chlorophenyl)-3-hydroxy-4-(1,2,4-(1H)-triazolyl)butane and 3.85 g (0.043 mol) of sodium 1,2,4-triazolide in 75 mL of dimethylformamide was stirred at room temperature for 28 hours. To this solution was added 200 mL of water and 200 mL of diethyl ether. The organic phase was separated from the aqueous phase and then washed thrice with 100 mL portions of water and then dried over anhydrous sodium sulfate. The solvent was removed by evaporation under reduced pressure to give a yellow oil which solidified on standing overnight. This material was recrystallized from benzene to give the above named product in a yield of 2.6 g (58 percent of theoretical), melting at 95°-99° C.

後処理

  1. customThe organic phase was separated from the aqueous phase
  2. washwashed thrice with 100 mL portions of water
  3. dry with materialdried over anhydrous sodium sulfate
  4. customThe solvent was removed by evaporation under reduced pressure
  5. customto give a yellow oil which
  6. customThis material was recrystallized from benzene
  7. customto give the above named product in a yield of 2.6 g (58 percent of theoretical), melting at 95°-99° C.

出典と根拠

ORDレコード
ord-212a24a344334edb992000b048c59209
出典データセット
uspto-grants-1990_05
特許番号
US04927833

反応ノート

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