Carbon tetrabromide → HCID 10858994, 화합물

HRID 260825노트

반응식

HRID 260825 반응식
[CH2:1]([C:5]1[CH:10]=[CH:9][C:8]([CH:11](O)[CH2:12][CH2:13][CH2:14][CH3:15])=[CH:7][CH:6]=1)[CH:2]([CH3:4])[CH3:3].C(Br)(Br)(Br)[Br:18].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>O1CCCC1>[Br:18][CH:11]([C:8]1[CH:9]=[CH:10][C:5]([CH2:1][CH:2]([CH3:4])[CH3:3])=[CH:6][CH:7]=1)[CH2:12][CH2:13][CH2:14][CH3:15]

참가 물질

5

반응물 3

HCID 11205Carbon tetrabromideHCID 11776TriphenylphosphineHCID 11790735HCID 11790735, 화합물

생성물 1

HCID 10858994HCID 10858994, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a mixture of 1-(4-isobutylphenyl)pentanol and carbon tetrabromide in tetrahydrofuran was added triphenylphosphine and the mixture was stirred at room temperature for 1 hour. Insoluble materials were removed by filtration and the filtrate was concentrated. Hexane was added to the residue and the mixture was filtered again. Concentration of the filtrate gave crude 1-bromo-1-(4-isobutylphenyl)pentane. Sodium was added portionwise to 1,3-propanediol at 80° C. while stirring. The obtained crude 1-bromo-1-(4-isobutylphenyl)pentane was added thereto, and the mixture was stirred at 120° C. for 30 minutes. After the mixture was cooled, diluted hydrochloric acid was added thereto, and the mixture was extracted with ethyl acetate.

후처리

  1. customInsoluble materials were removed by filtration
  2. concentrationthe filtrate was concentrated
  3. additionHexane was added to the residue
  4. filtrationthe mixture was filtered again

출처 및 근거

ORD 기록
ord-b6fdecfe883442f0a52649a6cce1c707
출처 데이터셋
uspto-grants-1996_06
특허 번호
US05530019

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