Carbon tetrabromide → HCID 12138359, 화합물

HRID 987178노트

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HRID 987178 반응식
[C:1]([C:5]1[CH:6]=[C:7]([CH:34]=[C:35]([C:37]([CH3:40])([CH3:39])[CH3:38])[CH:36]=1)[CH2:8][S:9][C:10]1[CH:11]=[C:12]([CH:15]=[C:16]([S:18][CH2:19][C:20]2[CH:25]=[C:24]([C:26]([CH3:29])([CH3:28])[CH3:27])[CH:23]=[C:22]([C:30]([CH3:33])([CH3:32])[CH3:31])[CH:21]=2)[CH:17]=1)[CH2:13]O)([CH3:4])([CH3:3])[CH3:2].C(Br)(Br)(Br)[Br:42].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>O1CCCC1>[C:1]([C:5]1[CH:6]=[C:7]([CH:34]=[C:35]([C:37]([CH3:40])([CH3:39])[CH3:38])[CH:36]=1)[CH2:8][S:9][C:10]1[CH:11]=[C:12]([CH:15]=[C:16]([S:18][CH2:19][C:20]2[CH:25]=[C:24]([C:26]([CH3:29])([CH3:28])[CH3:27])[CH:23]=[C:22]([C:30]([CH3:33])([CH3:32])[CH3:31])[CH:21]=2)[CH:17]=1)[CH2:13][Br:42])([CH3:4])([CH3:3])[CH3:2]

참가 물질

5

반응물 3

HCID 11205Carbon tetrabromideHCID 11776TriphenylphosphineHCID 12138358HCID 12138358, 화합물

생성물 1

HCID 12138359HCID 12138359, 화합물수율 64.1%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
27.5 °C

실험 절차

3,5-Bis(3,5-di-tertiary-butylbenzylthio)benzyl alcohol (49.0 g, 84.9 mmol) and carbon tetrabromide (28.2 g, 85.0 mmol) were dissolved in 300 ml of tetrahydrofuran. To this solution was added with stirring triphenylphosphin (23.5 g, 89.6 mmol), at the temperatures of 10° C. or below. The reaction mixture became clear once, and then colorless crystals separated gradually. After stirring overnight at 25-30° C., the crystals were removed by filtration and the filtrate was concentrated. The residue obtained was purified by means of chromatography with n-hexane:dichloromethane=1:1, giving 34.8 g of 3,5-bis(3,5-di-tertiary-butylbenzylthio)benzyl bromide.

후처리

  1. customcolorless crystals separated gradually
  2. customthe crystals were removed by filtration
  3. concentrationthe filtrate was concentrated
  4. customThe residue obtained
  5. customwas purified by means of chromatography with n-hexane

출처 및 근거

ORD 기록
ord-ac4e340ed43c46bba882cfd2604483eb
출처 데이터셋
uspto-grants-2003_10
특허 번호
US06630578B2

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