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Hydrochloric Acid → 6-Fluoro-2-oxobicyclo[3.1.0]hexane-6-carboxylic acid

HRID 2417313
ノート
印刷プレビュー

反応式

HRID 2417313 の反応式
[OH-].[Na+].[F:3][C:4]1([C:11]([O:13]CC)=[O:12])[CH:9]2[CH:5]1[CH2:6][CH2:7][C:8]2=[O:10].Cl>>[F:3][C:4]1([C:11]([OH:13])=[O:12])[CH:9]2[CH:5]1[CH2:6][CH2:7][C:8]2=[O:10]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 9964278Ethyl(1RS,5RS,6RS)-6-fluoro-2-oxobicyclo[3.1.0]hexane-6-carboxylate

生成物 1

HCID 226347796-Fluoro-2-oxobicyclo[3.1.0]hexane-6-carboxylic acid収率 103.9%

実験手順

A 1M aqueous solution of sodium hydroxide in an amount of 1.0 mL was added dropwise to 0.17 g of (1RS,5RS,6RS)ethyl 6-fluoro-2-oxobicyclo[3.1.0]hexane-6-carboxylate while being ice-cooled. The mixture was stirred for 2.5 hours at the same temperature. The pH of the reaction mixture was adjusted to 1 with concentrated hydrochloric acid, followed by extractions with chloroform three times. The organic layers were combined, and the combined organic layer was dried over anhydrous sodium sulfate. After the desiccant was filtered off, the filtrate was concentrated under reduced pressure, thereby yielding 0.15 g of (1RS,5RS,6RS)-6-fluoro-2-oxobicyclo[3.1.0]hexane-6-carboxylic acid.

このページの内容参加物実験手順後処理出典と根拠反応ノート

後処理

  1. temperaturecooled
  2. extractionfollowed by extractions with chloroform three times
  3. dry with materialthe combined organic layer was dried over anhydrous sodium sulfate
  4. filtrationAfter the desiccant was filtered off
  5. concentrationthe filtrate was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-fb26b8d515374bccafffc0dcd1248518
出典データセット
uspto-grants-2004_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06825375B2

反応ノート

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