反応 #213874

反応方程式

methyl ester

3-Carbomethoxymethyl-4-oxo-5-phthalimido-1,3-thiazine

tetrahydrofuran

hydrochloric acid

→

3-Carboxymethyl-4-oxo-5-phthalimido-1,3-thiazine

溶媒

water

反応条件

後処理

1. 1
   温度The solution was cooled
2. 2
   workup.ADDITIONdiluted with 5 ml
3. 3
   抽出of water and then extracted four times with a total of 15 ml
4. 4
   乾燥The organic phase was dried over sodium sulfate
5. 5
   濃縮concentrated in vacuo
6. 6
   その他The resulting residue was triturated with dichloromethane and crystals
7. 7
   その他formed
8. 8
   洗浄which were washed with dichloromethane
9. 9
   その他dried
10. 10
    その他to give 10.1 mg
11. 11
    濃縮The mother liquor on concentration in vacuo
12. 12
    その他also crystallized
13. 13
    その他to give 13.3 mg

実験手順

A 24 mg. (0.07 mmole) sample of the methyl ester product obtained in Step A. above, in a solution of 1.5 ml. of tetrahydrofuran, 0.5 ml. of water, and 0.25 ml. of concentrated hydrochloric acid, was refluxed under nitrogen for 3.5 hrs. The solution was cooled and diluted with 5 ml. of water and then extracted four times with a total of 15 ml. of dichloromethane. The organic phase was dried over sodium sulfate and concentrated in vacuo. The resulting residue was triturated with dichloromethane and crystals formed, which were washed with dichloromethane and dried to give 10.1 mg. of product having a m.p. of 227°-228° C. The mother liquor on concentration in vacuo also crystallized to give 13.3 mg. of product.

出典