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Hydrochloric Acid → 3-(1,1-Dimethylethyl)-4-(tetradecyloxy)benzoic acid

HRID 1728816
ノート
印刷プレビュー

反応式

HRID 1728816 の反応式
C[O:2][C:3](=[O:29])[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][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH3:24])=[C:6]([C:25]([CH3:28])([CH3:27])[CH3:26])[CH:5]=1.[OH-].[K+].Cl.C(Cl)(Cl)Cl>CO.C(O)C.O>[CH3:28][C:25]([C:6]1[CH:5]=[C:4]([CH:9]=[CH:8][C:7]=1[O:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH3:24])[C:3]([OH:29])=[O:2])([CH3:26])[CH3:27]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 313Hydrochloric AcidHCID 6212ChloroformHCID 14797Potassium HydroxideHCID 538584113-(1,1-Dimethylethyl)-4-(tetradecyloxy)benzoic acid methyl ester

生成物 1

HCID 190150743-(1,1-Dimethylethyl)-4-(tetradecyloxy)benzoic acid収率 88.7%

試薬・触媒・溶媒 3

HCID 702
Ethanol
溶媒
HCID 887Methanol溶媒
HCID 962Water溶媒

実験手順

A solution of 36.2 g Of product from Example 31 in 320 ml of methyl alcohol, 125 ml ethyl alcohol, 20 ml of water and 15 g of potassium hydroxide is mechanically stirred at reflux temperature for 41/2 hours. The reaction is cooled and 325 ml of 1N hydrochloric acid and 200 ml of chloroform is added. The mixture is heated until homogeneous, the layers are separated and extracted with chloroform. The combined organic layers are washed with 1N hydrochloric acid, dried and concentrated in vacuo. The residue is recrystallized from chloroform/hexane to give 31 g of the product as white crystals.

後処理

  1. temperatureat reflux temperature for 41/2 hours
  2. temperatureThe reaction is cooled
  3. temperatureThe mixture is heated until homogeneous, the layers
  4. customare separated
  5. extractionextracted with chloroform
  6. washThe combined organic layers are washed with 1N hydrochloric acid
  7. customdried
  8. concentrationconcentrated in vacuo
  9. customThe residue is recrystallized from chloroform/hexane

出典と根拠

ORDレコード
ord-a01bc04ae9e54614a2e08a6ef470f68c
出典データセット
uspto-grants-1994_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05328921

反応ノート

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