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

HRID 271347노트

반응식

HRID 271347 반응식
[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]

참가 물질

5

반응물 2

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

생성물 1

HCID 178451083HCID 178451083, 화합물수율 99.1%

시약·촉매·용매 2

HCID 23939Platinum촉매HCID 702Ethanol용매2회

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-95a0efb0825e4a77adb744b40e72c890
출처 데이터셋
uspto-grants-2008_11
특허 번호
US07452893B2

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