Hydrochloric Acid → 2-(4-ethoxybenzyloxy)-6,7-dihydro-5H-benzocycloheptene-8-carboxylic acid

HRID 1169336ノート

反応式

HRID 1169336 の反応式
[CH2:1]([O:3][C:4]1[CH:26]=[CH:25][C:7]([CH2:8][O:9][C:10]2[CH:11]=[CH:12][C:13]3[CH2:19][CH2:18][CH2:17][C:16]([C:20]([O:22]C)=[O:21])=[CH:15][C:14]=3[CH:24]=2)=[CH:6][CH:5]=1)[CH3:2].[OH-].[Na+].Cl>CO.C1COCC1>[CH2:1]([O:3][C:4]1[CH:26]=[CH:25][C:7]([CH2:8][O:9][C:10]2[CH:11]=[CH:12][C:13]3[CH2:19][CH2:18][CH2:17][C:16]([C:20]([OH:22])=[O:21])=[CH:15][C:14]=3[CH:24]=2)=[CH:6][CH:5]=1)[CH3:2]

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 22990168methyl 2-(4-ethoxybenzyloxy)-6,7-dihydro-5H-benzocycloheptene-8-carboxylate

生成物 1

HCID 229900572-(4-ethoxybenzyloxy)-6,7-dihydro-5H-benzocycloheptene-8-carboxylic acid収率 100%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8028Tetrahydrofuran溶媒

反応条件

温度
50 °C

実験手順

To methyl 2-(4-ethoxybenzyloxy)-6,7-dihydro-5H-benzocycloheptene-8-carboxylate (296 mg, 0.84 mmol) dissolved in a mixed solvent of methanol (4 ml) and THF (4 ml) was added a 1N aqueous solution of sodium hydroxide (2.5 ml), and the resulting mixture was stirred at 50° C. for 4 hours. The reaction mixture was mixed with 1 N hydrochloric acid (2.5 ml) at 0° C., was concentrated under reduced pressure and was mixed with water, and an insoluble material was collected by filtration. The insoluble material was washed with water, and was dried under reduced pressure to obtain 2-(4-ethoxybenzyloxy)-6,7-dihydro-5H-benzocycloheptene-8-carboxylic acid (283 mg, 0.84 mmol).

後処理

  1. concentrationwas concentrated under reduced pressure
  2. additionwas mixed with water
  3. filtrationan insoluble material was collected by filtration
  4. washThe insoluble material was washed with water
  5. customwas dried under reduced pressure

出典と根拠

ORDレコード
ord-db514b2ce172494fa75877df27b187ac
出典データセット
uspto-grants-2003_09
特許番号
US06627651B1

反応ノート

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