Potassium Carbonate → Ethyl 2-(m-tert-butyl-p-hydroxyphenoxy)tetradecanoate

HRID 1112077

反応式

HRID 1112077 の反応式
[C:1]([C:5]1[CH:11]=[C:10]([OH:12])[CH:9]=[CH:8][C:6]=1[OH:7])([CH3:4])([CH3:3])[CH3:2].Br[CH:14]([CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH3:31])[C:15]([O:17][CH2:18][CH3:19])=[O:16].C(=O)([O-])[O-].[K+].[K+]>CC(C)=O>[OH:7][C:6]1[CH:8]=[CH:9][C:10]([O:12][CH:14]([CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH3:31])[C:15]([O:17][CH2:18][CH3:19])=[O:16])=[CH:11][C:5]=1[C:1]([CH3:4])([CH3:2])[CH3:3]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 16043Tert-ButylhydroquinoneHCID 85791Tetradecanoic acid, 2-bromo-, ethyl ester

生成物 1

HCID 3015607Ethyl 2-(m-tert-butyl-p-hydroxyphenoxy)tetradecanoate収率 37.5%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

116 g of tert-butylhydroquinone, 234 g of ethyl α-bromotetradecanoate and 170 g of potassium carbonate were mixed in 1.6 liters of acetone and reacted for 48 hours under refluxing and stirring. After the reaction, the acetone was distilled off and the residue was dissolved in one liter of ethyl acetate. The organic solvent layer was washed with water, dried with sodium sulfate and concentrated. The residue was recrystallized from 250 ml of n-hexane to obtain 110 g of a white solid. The melting point was 45° to 48° C.

後処理

  1. customreacted for 48 hours
  2. temperatureunder refluxing
  3. customAfter the reaction
  4. distillationthe acetone was distilled off
  5. dissolutionthe residue was dissolved in one liter of ethyl acetate
  6. washThe organic solvent layer was washed with water
  7. dry with materialdried with sodium sulfate
  8. concentrationconcentrated
  9. customThe residue was recrystallized from 250 ml of n-hexane

出典と根拠

ORDレコード
ord-4c7b4f0e75604a328e7a60bee4c2460d
出典データセット
uspto-grants-1978_10
特許番号
US04120723

関連ノート

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