Trichloro-2-propen-1-ylsilane → HCID 57681726, 화합물

HRID 493460

반응식

HRID 493460 반응식
[CH2:1]([Si:4]([Cl:7])(Cl)Cl)[CH:2]=[CH2:3].N12CCCN=C1CCCCC2.[CH3:19][O:20][C:21]([CH3:32])([C@H:23]([OH:31])[C@@H:24]([OH:30])[C:25]([O:28][CH3:29])([CH3:27])[CH3:26])[CH3:22]>C(Cl)Cl>[CH2:1]([Si:4]1([Cl:7])[O:30][C@@H:24]([C:25]([O:28][CH3:29])([CH3:26])[CH3:27])[C@H:23]([C:21]([CH3:32])([O:20][CH3:19])[CH3:22])[O:31]1)[CH:2]=[CH2:3]

참가 물질

5

반응물 3

HCID 7867Trichloro-2-propen-1-ylsilaneHCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 11218000HCID 11218000, 화합물

생성물 1

HCID 57681726HCID 57681726, 화합물수율 44.5%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

Preparation of (4R,5R)-2-allyl-2-chloro-4,5-bis-(1-methoxy-1-methyl-[1,3,2]dioxasilolane: To a cooled (0° C.) solution of allyltrichlorosilane (7.0 mL; 48 mmol) in CH2Cl2 (80 mL) was added 1,8-diazabicyclo[5.4.0]undec-7-ene (15 mL; 102 mmol). A solution of (3R,4R)-2,5-dimethoxy-2,5-dimethyl-hexane-3,4-diol (10.0 g; 48 mmol) in CH2Cl2 (80 mL) was then added and the mixture was allowed to warm to ambient temperature and stirred for 12 hours. The solution was concentrated and the residue was treated with diethylether (100 mL). The mixture was stirred for 1 hour. The mixture was then filtered and the filtrate was concentrated. The residue was distilled under reduced pressure to give 6.6 g (44%) of (4R,5R)-2-allyl-2-chloro-4,5-bis-(1-methoxy-1-methyl-ethyl)-[1,3,2]dioxasilolane as a clear, colorless liquid.

후처리

  1. concentrationThe solution was concentrated
  2. additionthe residue was treated with diethylether (100 mL)
  3. stirringThe mixture was stirred for 1 hour
  4. filtrationThe mixture was then filtered
  5. concentrationthe filtrate was concentrated
  6. distillationThe residue was distilled under reduced pressure

출처 및 근거

ORD 기록
ord-75b0dd9355294c39a606712ebada1dd7
출처 데이터셋
uspto-grants-2009_05
특허 번호
US07534905B2

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