Bromocyclopentane → HCID 6484666、化合物

HRID 378969ノート

反応式

HRID 378969 の反応式
[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

参加物

6

反応物 3

HCID 8728BromocyclopentaneHCID 8991o-VanillinHCID 11430Potassium Carbonate

生成物 1

HCID 6484666HCID 6484666、化合物収率 615%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

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%).

後処理

  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)

出典と根拠

ORDレコード
ord-114a80d13eb54f2fb9c1fec91ebb6b9f
出典データセット
uspto-grants-2001_10
特許番号
US06297257B1

反応ノート

読み込み中…