Hydrogen Bromide → HCID 58999614, 화합물

HRID 1593612노트

반응식

HRID 1593612 반응식
[CH:1]12[O:7][CH:6]1[CH2:5][CH2:4][CH:3]([C:8]([O:10][CH2:11][CH3:12])=[O:9])[CH2:2]2.[BrH:13].C([O-])(O)=O.[Na+].C1(C)C=CC(S(O)(=O)=O)=CC=1>C(Cl)Cl.C1(C)C=CC=CC=1.O>[Br:13][CH:6]1[CH2:5][CH2:4][CH:3]([C:8]([O:10][CH2:11][CH3:12])=[O:9])[CH2:2][CH:1]1[OH:7]

참가 물질

8

반응물 4

HCID 260Hydrogen BromideHCID 6101p-Toluenesulfonic acidHCID 516892Sodium BicarbonateHCID 15691705Ethyl 7-oxabicyclo[4.1.0]heptane-3-carboxylate

생성물 1

HCID 58999614HCID 58999614, 화합물

시약·촉매·용매 3

HCID 962Water용매HCID 1140Toluene용매HCID 6344Dichloromethane용매

실험 절차

To a solution of ethyl 7-oxabicyclo[4.1.0]heptane-3-carboxylate (17.8 g) in CH2Cl2 (350 mL) was added 40% HBr solution (120 mL). The biphasic mixture was stirred vigorously for 25 min, then was neutralized with aqueous NaHCO3 solution. The organic layer was collected and dried over MgSO4, then was concentrated in vacuo. The residue was diluted with toluene (120 mL), and para-toluene sulfonic acid (120 mg, 0.6 mmol) was added. The mixture was heated at 128° C. with azeotropic removal of water over 3.5 hours, then was concentrated in vacuo to afford 21 g of a brown residue, which was used in the next reaction without purification.

후처리

  1. customThe organic layer was collected
  2. dry with materialdried over MgSO4
  3. concentrationwas concentrated in vacuo
  4. additionwas added
  5. concentrationwas concentrated in vacuo

출처 및 근거

ORD 기록
ord-8fc63e33d83649ca86448ba55bbb2949
출처 데이터셋
uspto-grants-2007_11
특허 번호
US07297704B2

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