Water → 1-(2-Bromoethyl)-6-methoxyindan

HRID 1977996

반응식

HRID 1977996 반응식
O[CH2:2][CH2:3][CH:4]1[C:12]2[C:7](=[CH:8][CH:9]=[C:10]([O:13][CH3:14])[CH:11]=2)[CH2:6][CH2:5]1.P(Br)(Br)[Br:16].O>ClCCl>[Br:16][CH2:2][CH2:3][CH:4]1[C:12]2[C:7](=[CH:8][CH:9]=[C:10]([O:13][CH3:14])[CH:11]=2)[CH2:6][CH2:5]1

참가 물질

5

반응물 3

HCID 962WaterHCID 24614Phosphorus tribromideHCID 109978572-(6-Methoxyindan-1-yl)ethanol

생성물 1

HCID 110971511-(2-Bromoethyl)-6-methoxyindan수율 27.4%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 1-(2-hydroxyethyl)-6-methoxyindan (4.95 g, 25.7 mmol) in dichloromethane (100 ml) was added dropwise at −5° C. phosphorus tribromide (0.86 ml, 2084 27.0 mmol). The mixture was stirred for 30 minutes. To the reaction mixture was added water, which was subjected to extraction with chloroform. The extract solution was washed with brine and dried over anhydrous magnesium sulfate, followed by distilling off the solvent under reduced pressure. The residue was purified by means of a silica gel column chromatography (hexane/ethyl acetate, 7:3→1:1) to give 1.80 g (yield 27%) of the above-titled compound as an oily product.

후처리

  1. extractionwas subjected to extraction with chloroform
  2. washThe extract solution was washed with brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. distillationby distilling off the solvent under reduced pressure
  5. customThe residue was purified by means of a silica gel column chromatography (hexane/ethyl acetate, 7:3→1:1)

출처 및 근거

ORD 기록
ord-a323d53e5f8a49fbac6123342e2eebbd
출처 데이터셋
uspto-grants-2001_05
특허 번호
US06235789B1

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