Bromocyclopentane → HCID 6484666, 화합물

HRID 378969노트

반응식

HRID 378969 반응식
[OH:1][C:2]1[C:9]([O:10][CH3:11])=[CH:8][CH:7]=[CH:6][C:3]=1[CH:4]=[O:5].C([O-])([O-])=O.[K+].[K+].[CH:18]1(Br)[CH2:22][CH2:21][CH2:20][CH2:19]1>C(O)C.O>[CH:18]1([O:1][C:2]2[C:9]([O:10][CH3:11])=[CH:8][CH:7]=[CH:6][C:3]=2[CH:4]=[O:5])[CH2:22][CH2:21][CH2:20][CH2:19]1

참가 물질

6

반응물 3

HCID 8728BromocyclopentaneHCID 8991o-VanillinHCID 11430Potassium Carbonate

생성물 1

HCID 6484666HCID 6484666, 화합물수율 615%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

A mixture of 2-hydroxy-3-methoxy-benzaldehyde (10 g, 6.57 mmoles), K2CO3 (18.16 g, 131 mmoles), cyclopentyl-bromide (14.05 ml, 131 mmoles) in absolute ethanol (150 ml) under nitrogen was refluxed under stirring for 55 hours. The mixture was diluted with water, thrice extracted in ethyl acetate, washed with water, anhydrified over Na2SO4 and evaporated to dryness, the yielded oil was purified by flash chromatography on silica gel (eluent petrolatum/ethyl acetate 95:5) to give 8.9 g of the title product (yield: 61%).

후처리

  1. temperaturewas refluxed
  2. extractionextracted in ethyl acetate
  3. washwashed with water
  4. customevaporated to dryness
  5. customthe yielded oil was purified by flash chromatography on silica gel (eluent petrolatum/ethyl acetate 95:5)

출처 및 근거

ORD 기록
ord-114a80d13eb54f2fb9c1fec91ebb6b9f
출처 데이터셋
uspto-grants-2001_10
특허 번호
US06297257B1

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