반응식
Br[C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[Cl:9].[OH-].[K+].[C:12]([OH:16])(=[O:15])[CH2:13][SH:14].ClSC(Cl)(C1C=CC=CC=1)C([O-])=O.ClC1C(Cl)=C(S)C=CC=1>CN1CCCC1=O>[Cl:9][C:3]1[CH:4]=[CH:5][C:6]([Cl:8])=[CH:7][C:2]=1[CH:13]([SH:14])[C:12]([OH:16])=[O:15]참가 물질
실험 절차
To a 500 ml flask equipped with a thermometer, a condenser and a stirrer were added 45.2 g (0.2 mol) of 1-bromo-2,5-dichlorobenzene, 23.7 g (0.4 mol) of 95% potassium hydroxide, 18.4 g (0.2 mol) of thioglycolic acid and 320 g of N-methyl-2-pyrrolidone, followed by stirring at 140° to 150° C. for 2 hours. Assay of the reaction solution by high performance liquid chromatography identified the solution as a mixture of dichlorophenylthioglycolate and dichlorothiophenol salt. Then, after distilling off the solvent, 300 g of water and 50 g of toluene were added for layer separation. To the water layer was added 45 g of concentrated hydrochloric acid, and the mixture was cooled to room temperature. The resulting crystal was filtered and dried to yield 28.7 g of 2,5-dichlorophenylthioglycolic acid. Its melting point was 129° to 131° C., and the yield was 60.5%. The results are given in Table 2.
후처리
- customTo a 500 ml flask equipped with a thermometer, a condenser and a stirrer
- distillationThen, after distilling off the solvent, 300 g of water and 50 g of toluene
- additionwere added for layer separation
- additionTo the water layer was added 45 g of concentrated hydrochloric acid
- filtrationThe resulting crystal was filtered
- customdried
출처 및 근거
- ORD 기록
- ord-a8496bce6d5e4e34bf39273275a81065
- 출처 데이터셋
- uspto-grants-1993_05
- 특허 번호
- US05210291
연결된 노트
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