반응식
[CH:1]([Cl:10])=[CH:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH3:9].[CH3:11][CH:12]=[CH:13][CH:14]=[CH:15]C.Cl[CH:18]([Cl:25])[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1>>[CH2:1]([Cl:10])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH:8]=[CH2:9].[CH2:18]([Cl:25])[CH2:19][CH2:24][CH2:23][CH2:22][CH2:21][CH2:20][CH:11]=[CH:12][CH3:13].[CH2:18]([Cl:25])[CH2:19][CH2:24][CH2:23][CH2:22][CH2:21][CH2:20][CH:11]=[CH:12][CH:13]=[CH:14][CH3:15]참가 물질
실험 절차
The so-produced nonenyl chloride (112 g; 700 mmol) was added to an equimolar amount of the 2,4-hexadiene in a 100 mL round-bottomed flask equipped with a magnetic stir bar and a reflux condenser, along with 6 g of α,α-dichlorotoluene. This solution was subsurface-sparged with nitrogen for 10 minutes. The catalyst of Example 1 (1.15 g; 1.4 mmol) was added and the reaction flask was placed in an 85° C. oil bath for 15 hours. The reaction was terminated by cooling to room temperature, followed by the addition of 300 ml of hexanes and filtering three times through 75 g of silica gel. Hexanes were removed under reduced pressure and the remaining liquid was vacuum distilled through a 2 cm×30 cm packed bed column to yield 12 g of 8-nonen-1-yl chloride (Bpt1.5 36-40° C.), 46.3 g of 8-decen-1-yl chloride (Bpt1.5 56-60° C.), 15.3 g of 8,10-dodecadien-1-yl chloride (Bpt1.5 90-91 C.), and 30.4 g of 76% purity 1,16-dichloro-8-hexadecene and high boilers that remained in the distillation pot.
후처리
- customThis solution was subsurface-sparged with nitrogen for 10 minutes
- customwas placed in an 85° C.
- customfor 15 hours
- customThe reaction was terminated
- additionfollowed by the addition of 300 ml of hexanes
- filtrationfiltering three times through 75 g of silica gel
- customHexanes were removed under reduced pressure
- distillationdistilled through a 2 cm×30 cm
출처 및 근거
- ORD 기록
- ord-337eee4613304a5ea5e9c311e21dd3d6
- 출처 데이터셋
- uspto-grants-1999_06
- 특허 번호
- US05916983
연결된 노트
불러오는 중…