Acetic Acid → 2-(2,4-Difluorophenyl)-3-(1,2,4-triazol-1-yl)-2-(trimethylsilyloxy)propane

HRID 725774

反応式

HRID 725774 の反応式
[O:1]1[C:3]([C:5]2[CH:10]=[CH:9][C:8]([F:11])=[CH:7][C:6]=2[F:12])([CH3:4])[CH2:2]1.[CH3:13][Si:14]([CH3:21])([CH3:20])N1C=NC=N1.[N:22]1([Na])[CH:26]=[N:25][CH:24]=[N:23]1.C(O)(=O)C>CN(C)C=O.O>[F:12][C:6]1[CH:7]=[C:8]([F:11])[CH:9]=[CH:10][C:5]=1[C:3]([O:1][Si:14]([CH3:21])([CH3:20])[CH3:13])([CH2:2][N:22]1[CH:26]=[N:25][CH:24]=[N:23]1)[CH3:4]

参加物

7

反応物 4

HCID 176Acetic AcidHCID 875581-Trimethylsilyl-1,2,4-triazoleHCID 197086482-(2,4-Difluorophenyl)-2-methyloxiraneHCID 178507090HCID 178507090、化合物

生成物 1

HCID 155169032-(2,4-Difluorophenyl)-3-(1,2,4-triazol-1-yl)-2-(trimethylsilyloxy)propane

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

5.13 g (0.03 moles) of 1,2-epoxy-2-(2,4-difluorophenyl)-propane are reacted with 6.35 g (0.045 moles) of 1-(trimethylsilyl)-1,2,4-triazole and 0.14 g (0.0015 moles) of 1,2,4-triazol-1-yl sodium in 40 ml of dimethyl formamide at 80° C. for 3 hours. Then the reaction mixture is cooled to room temperature, neutralized by glacial acetic acid, mixed with 200 ml of water and extracted twice with 50 ml of dichloromethane each. The combined extracts are washed three times with 50 ml of water each, dried over water-free sodium sulfate and evaporated in vacuo. After carrying out a separation as described in Example 5, removal of the solvent and crystallization from n-heptane 6.0 g (64.5%) of the title compound are obtained; m.p.: 51°-53° C.

後処理

  1. extractionextracted twice with 50 ml of dichloromethane each
  2. washThe combined extracts are washed three times with 50 ml of water each,
  3. dry with materialdried over water-free sodium sulfate
  4. customevaporated in vacuo
  5. customa separation
  6. customas described in Example 5, removal of the solvent and crystallization from n-heptane 6.0 g (64.5%) of the title compound
  7. customare obtained

出典と根拠

ORDレコード
ord-f1cd7047a8394a479c696b57110fd9b6
出典データセット
uspto-grants-1998_01
特許番号
US05707976

関連ノート

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