Hydrochloric Acid → HCID 21997570、化合物

HRID 1977259ノート

反応式

HRID 1977259 の反応式
Br[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][O:8][C:9]1[CH:18]=[CH:17][C:12]([C:13]([O:15][CH3:16])=[O:14])=[CH:11][CH:10]=1.[CH3:19][O-:20].[Na+].Cl>CO>[CH3:19][O:20][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][O:8][C:9]1[CH:18]=[CH:17][C:12]([C:13]([O:15][CH3:16])=[O:14])=[CH:11][CH:10]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 10942334Sodium MethoxideHCID 21997456HCID 21997456、化合物

生成物 1

HCID 21997570HCID 21997570、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

A solution of methyl 4-(6-bromo-n-hexyloxy)benzoate (186 g) in methanol (1 L) was treated with 28% sodium methoxide in methanol (340 ml) and the solution refluxed for 2 hours. After cooling, the stirred solution was adjusted to pH 2 with 1M-hydrochloric acid then extracted with ethyl acetate. The organic layer was washed with water, dried over magnesium sulfate, filtered and evaporated to give a crude oil. This oil was purified on a silica gel column (2 kg, 9:1 hexane-ethyl acetate elution) to give methyl 4-(6-methoxy-n-hexyloxy)benzoate (127 g) as an oil.

後処理

  1. temperaturethe solution refluxed for 2 hours
  2. temperatureAfter cooling
  3. extractionthen extracted with ethyl acetate
  4. washThe organic layer was washed with water
  5. dry with materialdried over magnesium sulfate
  6. filtrationfiltered
  7. customevaporated
  8. customto give a crude oil
  9. customThis oil was purified on a silica gel column (2 kg, 9:1 hexane-ethyl acetate elution)

出典と根拠

ORDレコード
ord-204068cd6dd44ce880ace9fed018fc57
出典データセット
uspto-grants-2001_05
特許番号
US06232290B1

反応ノート

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