Sodium Hydroxide → 2,4-Diiodo-6-mercaptophenol
反応式
[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]参加物
4
実験手順
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).
後処理
- 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
出典と根拠
- ORDレコード
- ord-3c26fa667aa840dba4bb46d5f6b0d7c2
- 出典データセット
- uspto-grants-1978_05
- 特許番号
- US04087445
反応ノート
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