Hydrogen Bromide → HCID 58999614、化合物

HRID 1593612ノート

反応式

HRID 1593612 の反応式
[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]

参加物

8

反応物 4

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

生成物 1

HCID 58999614HCID 58999614、化合物

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 1140Toluene溶媒HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-8fc63e33d83649ca86448ba55bbb2949
出典データセット
uspto-grants-2007_11
特許番号
US07297704B2

反応ノート

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