반응식
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([CH3:9])[C:6]([CH:10]=[CH:11][C:12]([CH3:22])=[CH:13][CH:14]=[CH:15][C:16]([CH3:21])=[CH:17][C:18]([OH:20])=[O:19])=[C:5]([CH3:23])[C:4]=1[CH3:24].P(Cl)(Cl)Cl.N1C=C[CH:32]=[CH:31][CH:30]=1.C(O)C#C>O1CCCC1.O>[CH2:32]([O:19][C:18](=[O:20])[CH:17]=[C:16]([CH3:21])[CH:15]=[CH:14][CH:13]=[C:12]([CH3:22])[CH:11]=[CH:10][C:6]1[C:7]([CH3:9])=[CH:8][C:3]([O:2][CH3:1])=[C:4]([CH3:24])[C:5]=1[CH3:23])[C:31]#[CH:30]참가 물질
반응물 4
생성물 1
시약·촉매·용매 2
실험 절차
20 g of 9-(4-methoxy-2,3,6-trimethyl-phenyl)-3,7-dimethyl-nona-2,4,6,8-tetraen-1-oic acid are dissolved in 200 ml of tetrahydrofuran. After the addition of 5.5 ml of phosphorus trichloride, the solution is stirred for 2 hours at room temperature, cooled to 0° C. and treated firstly with 50 ml of pyridine and then dropwise at 0°-5° C. with 50 ml of propargyl alcohol. The mixture is stirred for 2 hours at room temperature and then diluted with water. The organic phase is washed successively with water, dilute hydrochloric acid and a 2% aqueous sodium bicarbonate solution, dried over sodium sulphate and evaporated. There is obtained 9-(4-methoxy-2,3,6-trimethyl-phenyl)-3,7-dimethyl-nona-2,4,6,8-tetraen-1-oic acid propargyl ester which melts at 94°-95° C. after absorption on aluminium oxide using benzene as the eluent.
후처리
- temperaturecooled to 0° C.
- customdropwise at 0°-5° C.
- stirringThe mixture is stirred for 2 hours at room temperature
- washThe organic phase is washed successively with water, dilute hydrochloric acid
- dry with materiala 2% aqueous sodium bicarbonate solution, dried over sodium sulphate
- customevaporated
출처 및 근거
- ORD 기록
- ord-384e307aeb444726a21d904c1de3f699
- 출처 데이터셋
- uspto-grants-1985_07
- 특허 번호
- US04532355
연결된 노트
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