반응식
[Cl:1][C:2]1[CH:16]=[C:15]([O:17][CH2:18][CH:19]=[C:20]([Cl:22])[Cl:21])[CH:14]=[C:13]([Cl:23])[C:3]=1[O:4][CH2:5][CH2:6][CH2:7][CH2:8][O:9][CH2:10][CH:11]=O.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.Cl[C:44]([F:49])([F:48])C([O-])=O.[Na+].O>COCCOCCOC>[Cl:1][C:2]1[CH:16]=[C:15]([O:17][CH2:18][CH:19]=[C:20]([Cl:22])[Cl:21])[CH:14]=[C:13]([Cl:23])[C:3]=1[O:4][CH2:5][CH2:6][CH2:7][CH2:8][O:9][CH2:10][CH:11]=[C:44]([F:49])[F:48]참가 물질
반응물 4
생성물 1
시약·촉매·용매 1
반응 조건
- 온도
- 60 °C
실험 절차
A mixture of 1.21 g of 4-(2,6-dichloro-4-(3,3-dichloro-2-propenyloxy)phenoxy)butyloxyacetaldehyde, 0.87 g of triphenylphosphine and 10 ml of diglyme was stirred at 160° C., to which a solution (5 ml) of 0.69 g of sodium chlorodifluoroacetate in diglyme heated to 60° C. was added dropwise. After stirring at 160° C. for 1.5 hours, the reaction mixture was returned to room temperature, poured into water and extracted twice with 50 ml of diethyl ether. The diethyl ether layers Were combined, washed with water, dried over magnesium sulfate and then concentrated to give a crude product. The crude product was subjected to silica gel chromatography, which afforded 0.21 g of 3,5-dichloro-1-(3,3-dichloro-2-propenyloxy)-4-(4-(3,3-difluoro-2-propenyloxy)butyloxy)benzene (yield, 16%), nD23.0 1.5219.
후처리
- additionwas added dropwise
- customwas returned to room temperature
- extractionextracted twice with 50 ml of diethyl ether
- washwashed with water
- dry with materialdried over magnesium sulfate
- concentrationconcentrated
- customto give a crude product
출처 및 근거
- ORD 기록
- ord-a67d5650892d4378acaa41ca42f8aa1f
- 출처 데이터셋
- uspto-grants-2000_10
- 특허 번호
- US06140274
연결된 노트
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