Cyclobutanecarboxylic acid, 3-[2-(1,1-dimethylethoxy)-2-oxoethylidene]- → HCID 178451083、化合物

HRID 271347ノート

反応式

HRID 271347 の反応式
[C:1]([O:5][C:6]([CH:8]=[C:9]1[CH2:12][CH:11]([C:13]([OH:15])=[O:14])[CH2:10]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].[H][H]>[Pt].C(O)C>[C:1]([O:5][C:6]([CH2:8][C@@H:9]1[CH2:12][C@H:11]([C:13]([OH:15])=[O:14])[CH2:10]1)=[O:7])([CH3:4])([CH3:2])[CH3:3]

参加物

5

反応物 2

HCID 59834904Cyclobutanecarboxylic acid, 3-[2-(1,1-dimethylethoxy)-2-oxoethylidene]-HCID 178418361HCID 178418361、化合物

生成物 1

HCID 178451083HCID 178451083、化合物収率 99.1%

試薬・触媒・溶媒 2

HCID 23939Platinum触媒HCID 702Ethanol溶媒2 回

実験手順

A mixture of 2 g of 3-tert-butoxycarbonylmethylene-cyclobutanecarboxylic acid, 150 mL of ethanol, 0.5 g of 5% platinum on carbon, and 200 mL of ethanol was stirred under 1 atm of hydrogen for 48 h overnight, filtered, diluted with 20 mL of toluene and concentrated under reduced pressure. Drying under vacuum overnight gave 2 g of product, which was predominantly as a colorless oil: 1H NMR (400 MHz, CDCl3) 10.2 (br s, 1H), 3.0 (m, 1H), 2.3 (m, 1H), 2.38 (m, 4H), 2.0 (dd, 2H), 1.4 (s, 9).

後処理

  1. filtrationfiltered
  2. additiondiluted with 20 mL of toluene
  3. concentrationconcentrated under reduced pressure
  4. customDrying under vacuum overnight

出典と根拠

ORDレコード
ord-95a0efb0825e4a77adb744b40e72c890
出典データセット
uspto-grants-2008_11
特許番号
US07452893B2

反応ノート

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