Pyridine → HCID 19756480, 화합물

HRID 1587771노트

반응식

HRID 1587771 반응식
[C:1]([CH:3]([C:6]1[CH:11]=[CH:10][C:9]([Br:12])=[CH:8][CH:7]=1)[CH2:4]O)#[N:2].N1C=CC=CC=1.P(Br)(Br)[Br:20]>C(Cl)Cl>[C:1]([CH:3]([C:6]1[CH:11]=[CH:10][C:9]([Br:12])=[CH:8][CH:7]=1)[CH2:4][Br:20])#[N:2]

참가 물질

5

반응물 3

HCID 1049PyridineHCID 24614Phosphorus tribromideHCID 19756485HCID 19756485, 화합물

생성물 1

HCID 19756480HCID 19756480, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a mixture of 24 g (0.11 mol) 2-cyano-2-(4-bromophenyl)-ethanol and 4.5 g (0.055 mol) pyridine in 100 ml CH2Cl2 are slowly added, at -5° to 0°, 12 g (0.044 mol) PBr3. The mixture is stirred for 3 hours at room temperature, thereafter for 2 hours at 40°, allowed to cool off, then poured into 500 ml ice water and extracted with CH2Cl2. The extract is washed with water, dried and evaporated. The resulting residue is chromatographed over a silica gel column with hexane/diethylether 6:4. The glassy residue obtained after evaporation is worked up in toluene and thereafter ether to give the title compound in the form of a yellow powder, m.p. 171° (decomposing).

후처리

  1. additionare slowly added, at -5° to 0°
  2. waitfor 2 hours at 40°
  3. temperatureto cool off
  4. extractionextracted with CH2Cl2
  5. washThe extract is washed with water
  6. customdried
  7. customevaporated
  8. customThe resulting residue is chromatographed over a silica gel column with hexane/diethylether 6:4
  9. customThe glassy residue obtained
  10. customafter evaporation

출처 및 근거

ORD 기록
ord-8036ced249694ac989fedb2974d52246
출처 데이터셋
uspto-grants-1993_06
특허 번호
US05219876

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