반응식
Cl[CH2:2][CH2:3][C:4]([C:6]1[CH:7]=[C:8]2[C:13](=[CH:14][CH:15]=1)[C:12]([CH3:17])([CH3:16])[CH2:11][CH2:10][C:9]2([CH3:19])[CH3:18])=[O:5].C(N(CC)CC)C.[CH:27]([C:29]1[CH:38]=[CH:37][C:32]([C:33]([O:35][CH3:36])=[O:34])=[CH:31][CH:30]=1)=[O:28]>CN(C)C=O.[Cl-].C([N+]1C(C)=C(CCO)SC=1)C1C=CC=CC=1>[C:33]([C:32]1[CH:37]=[CH:38][C:29]([C:27](=[O:28])[CH2:2][CH2:3][C:4]([C:6]2[CH:15]=[CH:14][C:13]3[C:12]([CH3:17])([CH3:16])[CH2:11][CH2:10][C:9]([CH3:19])([CH3:18])[C:8]=3[CH:7]=2)=[O:5])=[CH:30][CH:31]=1)([O:35][CH3:36])=[O:34]참가 물질
반응물 3
생성물 1
시약·촉매·용매 2
실험 절차
5.6 g (0.02 mole) of 6-(3-chloropropionyl)-1,2,3,4-tetrahydro-1,1,4,4-tetramethylnapthalene and 3.3 ml (0.024 mole) of triethylamine in 30 ml of dimethylformamide were stirred for 1 hour at room temperature. Thereafter, a solution of 3.6 g (0.025 mole) of methyl 4-formylbenzoate and 1 g of 3-benzyl-5-(2-hydroxyethyl)-4-methylthiazolium chloride in 10 ml of dimethylformamide was added dropwise. Stirring was continued for 1 hour, after which the mixture was poured onto ice/water and extracted twice with ethyl acetate, and the combined organic extracts were washed several times with water, dried over magnesium sulfate and evaporated down. 3.7 g of 1-(4-carbomethoxyphenyl)-4-(5,6,7,8-tetrahydro-5,5,8,8-tetramethyl-2-naphthalenyl)-butane-1,4-dione of melting point 139°-141° C. were obtained from the residue (6.4 g) after recrystallization from ethanol.
후처리
- additionafter which the mixture was poured onto ice/water
- extractionextracted twice with ethyl acetate
- washthe combined organic extracts were washed several times with water
- dry with materialdried over magnesium sulfate
- customevaporated down
출처 및 근거
- ORD 기록
- ord-2d768b8697394d8b83e07f06b10a38a1
- 출처 데이터셋
- uspto-grants-1993_04
- 특허 번호
- US05206242
연결된 노트
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