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1,4-Dioxane → HCID 19811953, 화합물

HRID 373143
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HRID 373143 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 312751,4-DioxaneHCID 663334-Bromo-1,1,2-trifluorobut-1-eneHCID 178433997HCID 178433997, 화합물

생성물 1

HCID 19811953HCID 19811953, 화합물수율 54.5%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-86c55bdacd14474e82c0066a86653677
출처 데이터셋
uspto-grants-1992_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05162349

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