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Bromine → HCID 53657601, 화합물

HRID 1736496
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HRID 1736496 반응식
[C:1]([O:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=1[O:16][CH3:17])(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[Br:18]Br>C(O)(=O)C>[C:1]([O:9][C:10]1[CH:15]=[CH:14][C:13]([Br:18])=[CH:12][C:11]=1[O:16][CH3:17])(=[O:8])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 24408BromineHCID 682722-Methoxyphenyl benzoate

생성물 1

HCID 53657601HCID 53657601, 화합물

시약·촉매·용매 1

HCID 176Acetic Acid용매2회

실험 절차

A stirred solution of 2-methoxyphenyl benzoate (29.1 g) in glacial acetic acid (150 mL) is treated with a solution of bromine (7.2 mL) in glacial acetic acid (25 mL) during a period of 20 minutes, and the solution is then stirred for a further period of 30 minutes at room temperature. The mixture is concentrated in vacuo, and the resulting residue is dissolved in methyl t-butyl ether (200 mL), washed with water (100 mL) and saturated aqueous sodium bicarbonate solution (3×100 mL), dried over magnesium sulphate and evaporated. The resulting residue is recrystallized from cyclohexane, to give 4-bromo-2-methoxyphenyl benzoate (22.7), m.p. 73°-75° C. [Elemental analysis: C,55.0; H,3.6; Br, 25.5%; calculated: C,54.6; H,3.9; Br, 25.9%].

후처리

  1. concentrationThe mixture is concentrated in vacuo
  2. dissolutionthe resulting residue is dissolved in methyl t-butyl ether (200 mL)
  3. washwashed with water (100 mL) and saturated aqueous sodium bicarbonate solution (3×100 mL)
  4. dry with materialdried over magnesium sulphate
  5. customevaporated
  6. customThe resulting residue is recrystallized from cyclohexane

출처 및 근거

ORD 기록
ord-14b16b007a83493cb2e0a63e06704b74
출처 데이터셋
uspto-grants-1996_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05541219

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