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Ethanol → HCID 10590086, 화합물

HRID 2396259
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HRID 2396259 반응식
P(Br)(Br)[Br:2].[CH:5]([C:8]1[CH:15]=[C:14]([CH:16]([CH3:18])[CH3:17])[CH:13]=[C:12]([CH:19]([CH3:21])[CH3:20])[C:9]=1[CH2:10]O)([CH3:7])[CH3:6].CCO>CCOCC>[CH:5]([C:8]1[CH:15]=[C:14]([CH:16]([CH3:18])[CH3:17])[CH:13]=[C:12]([CH:19]([CH3:21])[CH3:20])[C:9]=1[CH2:10][Br:2])([CH3:7])[CH3:6]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 702EthanolHCID 24614Phosphorus tribromideHCID 10728422HCID 10728422, 화합물

생성물 1

HCID 10590086HCID 10590086, 화합물

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

A solution of PBr3 (2.7 g, 10 mmol) in ether (10 mL) was added slowly to a solution of 2,4,6-triisopropylbenzyl alcohol (4.68 g, 20 mmol) in 20 mL of ether at room temperature. The mixture was stirred for 1 hour, 5 mL of absolute EtOH was added, and stirring was continued for another 0.5 hour. The solvent was removed and the residue distributed between EtOAc and saturated Na2CO3. The EtOAc layer was separated, washed with brine, and dried over MgSO4. The solvent was evaporated and the pure product was isolated by column chromatography (100% CH2Cl2, 3.5 g, 59%); NMR (CDCl3): δ 1.2-1.4 (m, 18H), 2.8-3.0(m, 1H), 3.2-3.45 (m, 2H), 4.7 (s, 2H), 7.04 (s, 2H) ppm.

후처리

  1. stirringstirring
  2. waitwas continued for another 0.5 hour
  3. customThe solvent was removed
  4. customThe EtOAc layer was separated
  5. washwashed with brine
  6. dry with materialdried over MgSO4
  7. customThe solvent was evaporated
  8. customthe pure product was isolated by column chromatography (100% CH2Cl2, 3.5 g, 59%)

출처 및 근거

ORD 기록
ord-cb1b3fb6c9834b9a9e09e6033287c22e
출처 데이터셋
uspto-grants-1996_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05491172

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