Hydrochloric Acid → 4-(1,3-Dioxoisoindolin-2-yl)-1-methylcyclohexanecarboxylic acid

HRID 1944722ノート

反応式

HRID 1944722 の反応式
[O:1]=[C:2]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[C:4](=[O:11])[N:3]1[CH:12]1[CH2:17][CH2:16][C:15]([CH3:23])([C:18]([O:20]CC)=[O:19])[CH2:14][CH2:13]1.Cl>C(O)(=O)C>[O:1]=[C:2]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[C:4](=[O:11])[N:3]1[CH:12]1[CH2:17][CH2:16][C:15]([CH3:23])([C:18]([OH:20])=[O:19])[CH2:14][CH2:13]1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 58074352Ethyl 4-(1,3-dioxoisoindolin-2-yl)-1-methylcyclohexanecarboxylate2 回

生成物 1

HCID 580743564-(1,3-Dioxoisoindolin-2-yl)-1-methylcyclohexanecarboxylic acid収率 58%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
90 °C

実験手順

Ethyl 4-(1,3-dioxoisoindolin-2-yl)-1-methylcyclohexanecarboxylate (Intermediate 72, 900 mg, 2.85 mmol) was added to 6M aq. hydrochloric acid (0.951 mL, 5.71 mmol) in acetic acid (5 mL). The reaction mixture was heated to 90° C. for 48 h and then concentrated under vacuum. The residue was taken up in a minimal volume of ethyl acetate and a white solid precipitated. The solid was collected by filtration, washed with acetonitrile and dried to provide the product acid (475 mg) as a white solid. LCMS [M−H]=286.3

後処理

  1. concentrationconcentrated under vacuum
  2. customa white solid precipitated
  3. filtrationThe solid was collected by filtration
  4. washwashed with acetonitrile
  5. customdried

出典と根拠

ORDレコード
ord-c772fef17fdb4c969f22689298404ed5
出典データセット
uspto-grants-2013_03
特許番号
US08394858B2

反応ノート

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