반응식
C1OC2C(=CSC=2)[O:3]C1CO.[CH:12]1([N:18]=[C:19]=[N:20][CH:21]2[CH2:26][CH2:25][CH2:24][CH2:23][CH2:22]2)[CH2:17][CH2:16][CH2:15][CH2:14][CH2:13]1.C(C1C=CC(C2C=CC(OC(CCC)C(O)=O)=CC=2)=CC=1)#N>CN(C)C1C=CN=CC=1.C(Cl)Cl>[CH:21]1([NH:20][C:19]([NH:18][CH:12]2[CH2:13][CH2:14][CH2:15][CH2:16][CH2:17]2)=[O:3])[CH2:26][CH2:25][CH2:24][CH2:23][CH2:22]1참가 물질
실험 절차
2.20 g of a mixture of 80% of EDT-methanol and 20% of hydroxy-PDT (corresponding to 12.9 mmol; 10.3 mmol based on the main component EDT-methanol), 2.10 g (10.2 mmol) of N,N′-dicyclohexylcarbodiimide and 1 spatula tip of 4-(dimethylamino)pyridine are dissolved in 80 ml of CH2Cl2 and cooled in an ice bath. 3.00 g (10.2 mmol) of [(4′-cyano-1,1′-biphenyl-4-yl)oxy]valeric acid (see formula) are added a spatula at a time to the cold (0° C.) solution while stirring. Remaining [(4′-cyano-1,1′-biphenyl-4-yl)oxy]valeric acid is dissolved in 20 ml of CH2Cl2 and added to the reaction. After 1 hour, the reaction is continued at room temperature. After a further 48 hours, the colourless precipitate formed (N,N′-dicyclohexylurea) is filtered off. The clear, colourless solution is washed in succession with 3×75 ml of 1 N HCl, 3×75 ml of saturated NaHCO3 solution and 3×75 ml of saturated NaCl solution. The organic phase is dried over MgSO4, the desiccant is filtered off and the solvent is removed on a rotary evaporator. This gives 4.70 g of crude product.
후처리
- temperaturecooled in an ice bath
- additionadded to the reaction
- customis continued at room temperature
- waitAfter a further 48 hours
출처 및 근거
- ORD 기록
- ord-b8d4faafaf03445484dcc15e53710dff
- 출처 데이터셋
- uspto-grants-2009_09
- 특허 번호
- US07585983B2
연결된 노트
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