Water → 443982-73-8

HRID 2252344노트

반응식

HRID 2252344 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:8]=[C:9]([O:14][CH3:15])[C:10]=1[CH:11]([CH3:13])[CH3:12])[CH2:6]O.P(Br)(Br)[Br:17].O>CCOCC>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:8]=[C:9]([O:14][CH3:15])[C:10]=1[CH:11]([CH3:13])[CH3:12])[CH2:6][Br:17]

참가 물질

5

반응물 3

HCID 962WaterHCID 24614Phosphorus tribromideHCID 46928175(3,5-dimethoxy-4-propan-2-yl-phenyl)methanol

생성물 1

HCID 66842814443982-73-8수율 175.2%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

To 3,5-Dimethoxy-4-i-propylbenzyl alcohol (12.57 g, 59.8 mmol) in dry ether (100 mL) at 0° C. was added PBr3 (3.0 mL, 31.2 mmol) dropwise under nitrogen. The reaction was monitored by TLC. After the reaction was completed (˜4 h), water (180 mL) was added. The organic layer was separated and the aqueous layer was extracted with ether (3×50 mL). The extract was washed with water (20 mL), sat. Na2CO3 (20 mL), water (20 mL) and brine (20 mL), and dried over anhydrous sodium sulfate. Evaporation of the solution yielded pure bromide (14.93 g, 91.4%) as a white solid. 1HNMR (CDCl3, ppm): δ 1.29 (d, J=7.1 Hz, 6H), 3.64 (hept, J=7.1 Hz, 1H), 3.84 (s, 6H), 4.50 (s, 2H), 6.60 (s, 2H).

후처리

  1. additionwas added
  2. customThe organic layer was separated
  3. extractionthe aqueous layer was extracted with ether (3×50 mL)
  4. washThe extract was washed with water (20 mL), sat. Na2CO3 (20 mL), water (20 mL) and brine (20 mL)
  5. dry with materialdried over anhydrous sodium sulfate
  6. customEvaporation of the solution

출처 및 근거

ORD 기록
ord-142c063c6097424fb06b9f88b3fa8fef
출처 데이터셋
uspto-grants-2008_01
특허 번호
US07321050B2

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