反応 #60362

反応方程式

NaOAc

1-methyl-2,2,4-trioxo-1,2,3,4-tetrahydro-2λ6-benzo[c][1,2]thiazine-7-carboxylic acid methyl ester

hydroxylamine hydrochloride

→

title compound

4-hydroxyimino-1-methyl-2,2-dioxo-1,2,3,4-tetrahydro-2λ6-benzo[c][1,2]thiazine-7-carboxylic acid methyl ester

溶媒

EtOH

反応条件

後処理

1. 1
   温度After heating
2. 2
   温度at reflux for 4 days
3. 3
   その他it was evaporated
4. 4
   workup.ADDITIONdiluted with CH2Cl2 (400 mL)
5. 5
   洗浄washed with H2O
6. 6
   乾燥dried over MgSO4
7. 7
   ろ過filtered
8. 8
   濃縮concentrated in vacuo
9. 9
   その他Crystallization from MeOH

実験手順

NaOAc (3.66 g, 44.5 mmol) was added to an EtOH (100 mL) solution of 1-methyl-2,2,4-trioxo-1,2,3,4-tetrahydro-2λ6-benzo[c][1,2]thiazine-7-carboxylic acid methyl ester (4.00 g, 14.8 mmol) and hydroxylamine hydrochloride (1.55 g, 22.3 mmol). After heating at reflux for 4 days, it was evaporated, diluted with CH2Cl2 (400 mL), washed with H2O, dried over MgSO4, filtered, and concentrated in vacuo. Crystallization from MeOH provided the title compound. MS (−APCI, m/z): 283 (M−H)−.

出典