Ethyl 2-(3-(((tert-butoxy)carbonyl)amino)cyclobutylidene)acetate → Cyclobutaneacetic acid, 3-[[(1,1-dimethylethoxy)carbonyl]amino]-, ethyl ester

HRID 1855605ノート

反応式

HRID 1855605 の反応式
[C:1]([O:5][C:6]([NH:8][CH:9]1[CH2:12][C:11](=[CH:13][C:14]([O:16][CH2:17][CH3:18])=[O:15])[CH2:10]1)=[O:7])([CH3:4])([CH3:3])[CH3:2]>CO.[Pd]>[C:1]([O:5][C:6]([NH:8][CH:9]1[CH2:10][CH:11]([CH2:13][C:14]([O:16][CH2:17][CH3:18])=[O:15])[CH2:12]1)=[O:7])([CH3:4])([CH3:3])[CH3:2]

参加物

4

反応物 1

HCID 86701055Ethyl 2-(3-(((tert-butoxy)carbonyl)amino)cyclobutylidene)acetate

生成物 1

HCID 86701059Cyclobutaneacetic acid, 3-[[(1,1-dimethylethoxy)carbonyl]amino]-, ethyl ester収率 97.2%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

10% Pd/C (360 mg) was added to a solution of ethyl 2-(3-(tert-butoxycarbonylamino)cyclobutylidene)acetate (1.2 g, 4.8 mmol) in MeOH (10 mL) at 23° C. The reaction mixture was stirred under a H2 balloon at rt for 1.5 hrs. The mixture was filtered and concentrated. The residue was purified by silica gel column (10% EtOAc/petroleum ether) to afford ethyl 2-(3-(tert-butoxycarbonylamino)cyclobutyl)-acetate (1.2 g, 96%). ESI-MS (EI+, m/z): 258 [M+H]+.

後処理

  1. filtrationThe mixture was filtered
  2. concentrationconcentrated
  3. customThe residue was purified by silica gel column (10% EtOAc/petroleum ether)

出典と根拠

ORDレコード
ord-26bb08edcba34753bcec55c0d88d1269
出典データセット
uspto-grants-2015_02
特許番号
US08962844B2

反応ノート

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