Dimethylformamide → HCID 20489616、化合物

HRID 1995067ノート

反応式

HRID 1995067 の反応式
[K].[NH:2]1[CH:6]=[N:5][CH:4]=[N:3]1.[C:7]([C:11]1(CBr)[O:15][C:14]([CH3:25])([O:16][C:17]2[CH:22]=[CH:21][C:20]([Cl:23])=[CH:19][C:18]=2[Cl:24])[CH2:13][O:12]1)([CH3:10])([CH3:9])[CH3:8].[CH3:28]N(C)C=O>>[C:7]([C:11]1([N:2]2[CH:6]=[N:5][CH:4]=[N:3]2)[O:15][C:14]([CH3:25])([O:16][C:17]2[CH:22]=[CH:21][C:20]([Cl:23])=[CH:19][C:18]=2[Cl:24])[CH:13]([CH3:28])[O:12]1)([CH3:8])([CH3:9])[CH3:10]

参加物

4

反応物 3

HCID 6228Dimethylformamide2 回HCID 20489617HCID 20489617、化合物HCID 534465811,2,4-Triazole potassium

生成物 1

HCID 20489616HCID 20489616、化合物

実験手順

3.5 g of 1,2,4-triazole potassium salt in 100 ml of absolute dimethylformamide are heated to 100°. To the hot solution are added dropwise 9 g of 2-tert-butyl-2-bromomethyl-4-(2,4-dichlorophenoxy)-methyl-1,3-dioxolane dissolved in 50 ml of absolute dimethylformamide. The reaction mixture is subsequently stirred for 24 hours at 130°; the solvent is then removed in vacuo and the residue is extracted with diethyl ether; the ether phase is washed with water and dried over sodium sulfate. The yield after concentration by evaporation is 7 g of a viscous oil which, after the addition of n-hexane, crystallises to give the cis isomer, m.p. 113°-114°. The trans isomer, m.p. 73°-74°, can be obtained from the mother liquor.

後処理

  1. customthe solvent is then removed in vacuo
  2. extractionthe residue is extracted with diethyl ether
  3. washthe ether phase is washed with water
  4. dry with materialdried over sodium sulfate
  5. customThe yield
  6. concentrationafter concentration
  7. customby evaporation
  8. additionafter the addition of n-hexane
  9. customcrystallises
  10. customto give the cis isomer, m.p. 113°-114°
  11. customThe trans isomer, m.p. 73°-74°, can be obtained from the mother liquor

出典と根拠

ORDレコード
ord-908baca882254dbc8b7bfd8e2dff1c28
出典データセット
uspto-grants-1983_09
特許番号
US04402963

反応ノート

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