Hydrochloric Acid → 5-Hexene-1,2,3-triol
반응식
CC1(C)[O:6][CH:5]([CH:7]([CH2:9][CH:10]=[CH2:11])[OH:8])[CH2:4][O:3]1.Cl.C(Cl)(Cl)Cl>O1CCCC1>[CH2:4]([OH:3])[CH:5]([OH:6])[CH:7]([OH:8])[CH2:9][CH:10]=[CH2:11]참가 물질
5
실험 절차
A solution of 11 g of [R-(R*,R*)]-2,2-dimethyl-alpha-2-propenyl-1,3-dioxolane-4-methanol, prepared by the procedure described in J. Am. Chem. Soc., 1985, 107(26), 8186-8190, in 300 ml of 1:1 tetrahydrofuran: 2N hydrochloric acid is heated at the reflux temperature of the solvents for 2 hours. Chloroform is added and the layers are separated. The aqueous layer is re-extracted 2X with chloroform. The aqueous layer is neutralized with potassium carbonate and exhaustively extracted with 80% chloroform/iso-propanol. Thecombined organic layers are concentrated in vacuo to give 7.51 g of the desired product.
후처리
- customthe layers are separated
- extractionThe aqueous layer is re-extracted 2X with chloroform
- extractionexhaustively extracted with 80% chloroform/iso-propanol
- concentrationThecombined organic layers are concentrated in vacuo
출처 및 근거
- ORD 기록
- ord-274fb1655ec945eea31aa375d8b09370
- 출처 데이터셋
- uspto-grants-1998_04
- 특허 번호
- US05744465
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