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1,4-Dioxane → HCID 19811953、化合物

HRID 373143
ノート
印刷プレビュー

反応式

HRID 373143 の反応式
[SH:1][C:2]1[O:3][C:4]([C:7]2[O:11][C:10]([CH3:12])=[N:9][N:8]=2)=[N:5][N:6]=1.O1CCOCC1.Br[CH2:20][CH2:21][C:22]([F:26])=[C:23]([F:25])[F:24]>CN(C)C=O>[F:26][C:22](=[C:23]([F:25])[F:24])[CH2:21][CH2:20][S:1][C:2]1[O:3][C:4]([C:7]2[O:11][C:10]([CH3:12])=[N:9][N:8]=2)=[N:5][N:6]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 312751,4-DioxaneHCID 663334-Bromo-1,1,2-trifluorobut-1-eneHCID 178433997HCID 178433997、化合物

生成物 1

HCID 19811953HCID 19811953、化合物収率 54.5%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

3.7 g of 2-mercapto-5-(2-methyl-1,3,4-oxadiazol-5-yl)-1,3,4-oxadiazole according to Example H1 are initially introduced into a mixture of 36 ml of dioxane and 4 ml of dimethylformamide, and 2.24 g of potassium t-butylate are added, while stirring. 4.2 g of 4-bromo-1,1,2-trifluorobut-1-ene are added dropwise and the mixture is stirred overnight at room temperature. After the salts have been filtered off, the solvents are distilled off in vacuo, the residue is taken up in methylene chloride, the solution is washed with water and 1-normal sodium hydroxide solution in succession and the solvent is evaporated off in vacuo. 3.2 g of the desired compound of melting point 77°-79° C. are obtained as the residue.

後処理

  1. additionare added
  2. stirringthe mixture is stirred overnight at room temperature
  3. filtrationAfter the salts have been filtered off
  4. distillationthe solvents are distilled off in vacuo
  5. washthe solution is washed with water and 1-normal sodium hydroxide solution in succession
  6. customthe solvent is evaporated off in vacuo

出典と根拠

ORDレコード
ord-86c55bdacd14474e82c0066a86653677
出典データセット
uspto-grants-1992_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05162349

反応ノート

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