Carbon tetrabromide → HCID 12138359, 화합물

HRID 1271669노트

반응식

HRID 1271669 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

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-455ff5c9c50f470ba3fb644976b24a50
출처 데이터셋
uspto-grants-2007_04
특허 번호
US07205428B2

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