Hydrochloric Acid → 2-Oxobicyclo(3.1.0)hexane-6-carboxylic acid

HRID 1766

反応式

HRID 1766 の反応式
[O:1]=[C:2]1[CH2:7][CH2:6][CH:5]2[CH:3]1[CH:4]2[C:8]([O:10]CC)=[O:9].Cl>[OH-].[Na+]>[O:1]=[C:2]1[CH2:7][CH2:6][CH:5]2[CH:3]1[CH:4]2[C:8]([OH:10])=[O:9]

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 565357Ethyl 2-oxobicyclo[3.1.0]hexane-6-carboxylate

生成物 1

HCID 102194732-Oxobicyclo(3.1.0)hexane-6-carboxylic acid

試薬・触媒・溶媒 1

HCID 14798Sodium Hydroxide溶媒

実験手順

A mixture of 60 g of ethyl 2-oxobicyclo[3.1.0]hexane-6-carboxylate and 300 ml of 1N sodium hydroxide was stirred at 25°-30° C. After 2.5 hours, concentrated hydrochloric acid was added to adjust the pH to 0.8-1.2. The resulting solution was extracted with ethyl acetate. The extracts were dried over magnesium sulfate, filtered, and concentrated to give 49.1 g (98%) of the crude material. Recrystallization from 100 ml of ethyl acetate gave the title compound, mp 123.5°-128° C.

後処理

  1. extractionThe resulting solution was extracted with ethyl acetate
  2. dry with materialThe extracts were dried over magnesium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customto give 49.1 g (98%) of the crude material
  6. customRecrystallization from 100 ml of ethyl acetate

出典と根拠

ORDレコード
ord-07beb0ec388f43cd9ac71486ee726a73
出典データセット
uspto-grants-1998_03
特許番号
US05726320

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