반응 #50443
ord-5db9dc541d104704a857d69cebb76a01
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반응 조건
상세 조건
See reaction.notes.procedure_details.
후처리
- 1workup.ADDITIONthe whole is treated dropwise at from -7° to -3° C.
- 2기타the crystals which have separated
- 3여과are then filtered off
- 4세척They are washed with water
- 5기타recrystallised from acetone/n-hexane
실험 절차
1.0 g of 7-[(4,6-dimethoxy-pyrimidin-2-yl)oxy]-3-hydroxy-phthalide (see Example 84) is introduced into a solution of 2.1 g of potassium cyanide in 15 ml of water and the whole is treated dropwise at from -7° to -3° C., with cooling, over a period of 10 minutes, with 10 ml of concentrated hydrochloric acid. It is subsequently stirred at room temperature for approximately 16 hours and the crystals which have separated are then filtered off. They are washed with water and recrystallised from acetone/n-hexane to yield 0.2 g of 3-carbamoyl-7-[(4,6-dimethoxy-pyrimidin-2-yl)oxy]-phthalide (see also Example 17).