Potassium Hydroxide → 3-[4-(5-tert-Butyl-2-methyl-phenylethynyl)-phenyl]-acrylic acid

HRID 1869953ノート

反応式

HRID 1869953 の反応式
C([O:3][C:4](=[O:26])[CH:5]=[CH:6][C:7]1[CH:12]=[CH:11][C:10]([C:13]#[C:14][C:15]2[CH:20]=[C:19]([C:21]([CH3:24])([CH3:23])[CH3:22])[CH:18]=[CH:17][C:16]=2[CH3:25])=[CH:9][CH:8]=1)C.[OH-].[K+]>C(O)C.O1CCCC1>[C:21]([C:19]1[CH:18]=[CH:17][C:16]([CH3:25])=[C:15]([C:14]#[C:13][C:10]2[CH:11]=[CH:12][C:7]([CH:6]=[CH:5][C:4]([OH:26])=[O:3])=[CH:8][CH:9]=2)[CH:20]=1)([CH3:24])([CH3:23])[CH3:22]

参加物

5

反応物 2

HCID 14797Potassium HydroxideHCID 690739133-[4-(5-tert-Butyl-2-methyl-phenylethynyl)-phenyl]-acrylic acid ethyl ester2 回

生成物 1

HCID 690781133-[4-(5-tert-Butyl-2-methyl-phenylethynyl)-phenyl]-acrylic acid収率 77.3%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of 3-[4-(5-tert-butyl-2-methyl-phenylethynyl)-phenyl]-acrylic acid ethyl ester (Intermediate 111, 0.09 g, 0.26 mmol) in ethanol (3 mL) and tetrahydrofuran (3 mL) was treated with 3M potassium hydroxide solution (1 mL, 3 mmol) and the resulting reaction mixture was stirred overnight at ambient temperature. The reaction mixture was concentrated in vacuo slightly, the residue was neutralized with dilute hydrochloric acid, and the solid that was formed was filtered and washed with water and acetonitrile and dried to afford title product (0.064 g, 77%).

後処理

  1. customthe resulting reaction mixture
  2. concentrationThe reaction mixture was concentrated in vacuo slightly
  3. customthe solid that was formed
  4. filtrationwas filtered
  5. washwashed with water and acetonitrile
  6. customdried

出典と根拠

ORDレコード
ord-6ce1953cc3364846b519d517b3f271b6
出典データセット
uspto-grants-2009_12
特許番号
US07638648B2

反応ノート

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