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

HRID 1169326
ノート
印刷プレビュー

反応式

HRID 1169326 の反応式
[C:1]1([C:7]2[CH:29]=[CH:28][C:10]([CH2:11][O:12][C:13]3[CH:14]=[CH:15][C:16]4[CH2:22][CH2:21][CH2:20][C:19]([C:23]([O:25]C)=[O:24])=[CH:18][C:17]=4[CH:27]=3)=[CH:9][CH:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[OH-].[Na+].Cl>CO.C1COCC1>[C:1]1([C:7]2[CH:8]=[CH:9][C:10]([CH2:11][O:12][C:13]3[CH:14]=[CH:15][C:16]4[CH2:22][CH2:21][CH2:20][C:19]([C:23]([OH:25])=[O:24])=[CH:18][C:17]=4[CH:27]=3)=[CH:28][CH:29]=2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=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 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 22990066methyl 2-(4-phenylbenzyloxy)-6,7-dihydro-5H-benzocycloheptene-8-carboxylate

生成物 1

HCID 229901402-(4-phenylbenzyloxy)-6,7-dihydro-5H-benzocycloheptene-8-carboxylic acid収率 117.5%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒
HCID 8028
Tetrahydrofuran
溶媒

反応条件

温度
60 °C

実験手順

To methyl 2-(4-phenylbenzyloxy)-6,7-dihydro-5H-benzocycloheptene-8-carboxylate (1.22 g, 3.17 mmol) dissolved in a mixed solvent of methanol (20 ml) and THF (35 ml) was added a 1N aqueous solution of sodium hydroxide (10 ml), and the resulting mixture was stirred at room temperature for 18 hours and 60° C. for 2 hours. The reaction mixture was mixed with 1 N hydrochloric acid (12 ml) at room temperature, was concentrated under reduced pressure and was mixed with water, and an insoluble material was collected by filtration. The insoluble material was washed successively with water and hexane, and was dried under reduced pressure to obtain 2-(4-phenylbenzyloxy)-6,7-dihydro-5H-benzocycloheptene-8-carboxylic acid (1.38 g).

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 successively with water and hexane
  5. customwas dried under reduced pressure

出典と根拠

ORDレコード
ord-825508ac58c4459997b092f9f123e638
出典データセット
uspto-grants-2003_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06627651B1

反応ノート

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