Sodium Hydroxide → 2,4-Diiodo-6-mercaptophenol
반응식
[I-].[I:2][C:3]1[CH:4]=[C:5]([I:15])[C:6]2[O:10]C(=[N+](C)C)[S:8][C:7]=2[CH:14]=1.[OH-].[Na+]>CO>[I:15][C:5]1[CH:4]=[C:3]([I:2])[CH:14]=[C:7]([SH:8])[C:6]=1[OH:10]참가 물질
4
실험 절차
An amount of 13 g (23.3 m mol) of N-(5,7-diiodo-1,3-benzoxathiol-2-ylidene)-N-methylmethanaminium iodide was heated at reflux for 4 hours in a mixture of 200 ml of methanol and 50 ml of aqueous 10 percent sodium hydroxide. The reaction mixture was filtered, added to 400 ml of water and acidified with hydrochloric acid. The mixture was extracted with methylene chloride. After drying over anhydrous sodium sulfate, the methylene chloride extract was condensed in vacuo to give 6.1 g (69.4 percent yield) of 2,4-diiodo-6-mercaptophenol: M.P. 177.5°-179.5° C; nmr (DMSO-d6) δ 7.96 (doublet), 7.57 (doublet), and 3.42 (broad singlet).
후처리
- filtrationThe reaction mixture was filtered
- additionadded to 400 ml of water
- extractionThe mixture was extracted with methylene chloride
- dry with materialAfter drying over anhydrous sodium sulfate
- extractionthe methylene chloride extract
- customcondensed in vacuo
출처 및 근거
- ORD 기록
- ord-3c26fa667aa840dba4bb46d5f6b0d7c2
- 출처 데이터셋
- uspto-grants-1978_05
- 특허 번호
- US04087445
반응 노트
불러오는 중…