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Phosphorus tribromide → 1,3-Dithiolane, 4-bromomethyl-2-phenyl-

HRID 1605064
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인쇄 미리보기

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HRID 1605064 반응식
O[CH2:2][CH:3]1[CH2:7][S:6][CH:5]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[S:4]1.P(Br)(Br)[Br:15].C([O-])(O)=O.[Na+]>CCOCC>[Br:15][CH2:2][CH:3]1[CH2:7][S:6][CH:5]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[S:4]1
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참가 물질

5

반응물 3

HCID 24614Phosphorus tribromideHCID 474291HCID 474291, 화합물HCID 516892Sodium Bicarbonate

생성물 1

HCID 370591,3-Dithiolane, 4-bromomethyl-2-phenyl-수율 99%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

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온도
0 °C

실험 절차

4-Hydroxymethyl 2-phenyl 1,3-dithiolane (30 g., 0.14 mole) was suspended in 150 ml of ether and cooled to 0°C. Phosphorus tribromide (15 g., 0.053 mole) were added over a 1.5 hour period and the mixture was stirred at ambient temperature with 5% aqueous NaHCO3 until neutral (ph = 7). After drying over MgSO4 the solvent was removed under vacuum to yield 38 g. (99%) of desired product.

후처리

  1. dry with materialAfter drying over MgSO4 the solvent
  2. customwas removed under vacuum
  3. customto yield 38 g

출처 및 근거

ORD 기록
ord-9993c761b10e4d94a5509ca8e7140f1c
출처 데이터셋
uspto-grants-1976_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03948944

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