Pyridine → HCID 18950366, 화합물

HRID 1492378노트

반응식

HRID 1492378 반응식
N1C=CC=CC=1.[C:7]1([CH2:13][C:14]#[C:15][CH2:16]O)[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1.P(Br)(Br)[Br:19]>C1(C)C=CC=CC=1>[Br:19][CH2:16][C:15]#[C:14][CH2:13][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1

참가 물질

5

반응물 3

HCID 1049PyridineHCID 24614Phosphorus tribromideHCID 12474205HCID 12474205, 화합물

생성물 1

HCID 18950366HCID 18950366, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

14.5 ml of pyridine were added to a mixture of 140.4 g (0.96 mol) of 4-phenyl-2-butyn-1-ol (prepared according to G. Dupont, Bull. Soc. Chim. Fr., 1954, page 816) and 600 ml of dry toluene, after which 119.1 g (0.44 mol) of phosphorus tribromide were added dropwise in the course of 2 hours, the temperature not being allowed to exceed 50° C. The mixture was stirred overnight at room temperature and then poured onto 1,000 ml of ice water, the organic phase was separated off and the aqueous phase was extracted several times with methyl tert-butyl ether. The combined organic phases were then washed neutral and dried. The crude product obtained after the solvent had been stripped off under reduced pressure was subjected to fractional distillation. Yield: 126 g of product having a purity of 93% according to gas chromatography; bp.: 83°-85° C. at 0.3 mbar.

후처리

  1. customto exceed 50° C
  2. customthe organic phase was separated off
  3. extractionthe aqueous phase was extracted several times with methyl tert-butyl ether
  4. washThe combined organic phases were then washed neutral
  5. customdried

출처 및 근거

ORD 기록
ord-2c6fc94e6ba2477bbf53da57998cd8da
출처 데이터셋
uspto-grants-1994_12
특허 번호
US05374609

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