Potassium Carbonate → Methyl 4-(octyloxy)-2-[(pent-4-en-1-yl)oxy]benzoate

HRID 2220007

反応式

HRID 2220007 の反応式
[CH3:1][O:2][C:3](=[O:20])[C:4]1[CH:9]=[CH:8][C:7]([O:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH3:18])=[CH:6][C:5]=1[OH:19].Br[CH2:22][CH2:23][CH2:24][CH:25]=[CH2:26].C([O-])([O-])=O.[K+].[K+]>CC(=O)CC>[CH3:1][O:2][C:3](=[O:20])[C:4]1[CH:9]=[CH:8][C:7]([O:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH3:18])=[CH:6][C:5]=1[O:19][CH2:26][CH2:25][CH2:24][CH:23]=[CH2:22]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 707041-Pentene, 5-bromo-HCID 11536459Methyl 2-hydroxy-4-octyloxybenzoate

生成物 1

HCID 69309676Methyl 4-(octyloxy)-2-[(pent-4-en-1-yl)oxy]benzoate

試薬・触媒・溶媒 1

HCID 6569Methyl Ethyl Ketone溶媒

実験手順

A mixture of 66.1 g (0.234 mol) of 2-Hydroxy-4-octyloxy benzoic acid methyl ester obtained in Step 1, 44.7 g (0.30 mol) of 5-Bromopent-1-ene, 207 g (1.5 mol) of K2CO3 and 700 mL of dry butanone is refluxed for 24 h, then allowed to return to room temperature. The reaction mixture is filtered and the butanone is distilled off under reduced pressure. After drying the residue under vacuum a slightly yellow oil (77.5 g, 95%) is obtained, which can be used in the next step without further purification.

後処理

  1. temperatureis refluxed for 24 h
  2. customto return to room temperature
  3. filtrationThe reaction mixture is filtered
  4. distillationthe butanone is distilled off under reduced pressure
  5. dry with materialAfter drying the residue under vacuum a slightly yellow oil (77.5 g, 95%)
  6. customis obtained
  7. customwhich can be used in the next step without further purification

出典と根拠

ORDレコード
ord-de0158ce895c4d5dafc86eded8a4cfff
出典データセット
uspto-grants-2008_08
特許番号
US07416682B2

関連ノート

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