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Potassium Carbonate → HCID 17817500、化合物

HRID 1356442
ノート
印刷プレビュー

反応式

HRID 1356442 の反応式
C([CH:3]([C:7]1[CH:12]=[CH:11][C:10]([OH:13])=[CH:9][CH:8]=1)[C:4]([OH:6])=[O:5])C.C(=O)([O-])[O-].[K+].[K+].[C:20]1([C:26]2[CH:33]=[CH:32][C:29]([CH2:30]Cl)=[CH:28][CH:27]=2)[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1>CN(C=O)C.C(OCC)(=O)C>[C:26]1([C:20]2[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=2)[CH:27]=[CH:28][C:29]([CH2:30][O:13][C:10]2[CH:9]=[CH:8][C:7]([CH2:3][C:4]([OH:6])=[O:5])=[CH:12][CH:11]=2)=[CH:32][CH:33]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 11430Potassium CarbonateHCID 154634-Phenylbenzyl chlorideHCID 34656alpha-Ethyl-4-hydroxybenzeneacetic acid

生成物 1

HCID 17817500HCID 17817500、化合物収率 84.4%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate
溶媒

反応条件

温度
60 °C

実験手順

To a solution of ethyl 4-hydroxyphenylacetic acid (3.6 g) in DMF (50 ml) were added potassium carbonate (2.5 g) and 4-phenylbenzyl chloride (4 g) sequentially. After stirring at 60° C. for 6 hr, the reaction mixture was poured onto water and the resulting crystals were suspended in ethyl acetate. The suspension was washed with water and concentrated. The resulting crude crystals were dissolved in THF (100 ml)/ethanol (50 ml) and 2 N sodium hydroxide (20 ml) was added to the solution. The reaction mixture was heated under stirring at 60° C. for 18 hr and concentrated. The residue was acidified with 2 N hydrochloric acid and the resulting crystals were collected by filtration and washed with ethyl ether to obtain the titled compound (5.3 g).

後処理

  1. additionthe reaction mixture was poured onto water
  2. washThe suspension was washed with water
  3. concentrationconcentrated
  4. dissolutionThe resulting crude crystals were dissolved in THF (100 ml)/ethanol (50 ml) and 2 N sodium hydroxide (20 ml)
  5. additionwas added to the solution
  6. temperatureThe reaction mixture was heated
  7. stirringunder stirring at 60° C. for 18 hr
  8. concentrationconcentrated
  9. filtrationthe resulting crystals were collected by filtration
  10. washwashed with ethyl ether

出典と根拠

ORDレコード
ord-3463aa3e011240a0ae764ab68a912486
出典データセット
uspto-grants-2003_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06586475B1

反応ノート

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