Hydrazine hydrate (1:1) → HCID 86701057、化合物

HRID 1855606ノート

反応式

HRID 1855606 の反応式
[C:1]([O:5][C:6]([NH:8][CH:9]1[CH2:12][CH:11]([CH2:13][C:14]([O:16]CC)=O)[CH2:10]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].O.[NH2:20][NH2:21]>CCO>[NH:20]([C:14](=[O:16])[CH2:13][CH:11]1[CH2:12][CH:9]([NH:8][C:6](=[O:7])[O:5][C:1]([CH3:4])([CH3:3])[CH3:2])[CH2:10]1)[NH2:21]

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 86701059Cyclobutaneacetic acid, 3-[[(1,1-dimethylethoxy)carbonyl]amino]-, ethyl ester

生成物 1

HCID 86701057HCID 86701057、化合物収率 97%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of ethyl 2-(3-(tert-butoxycarbonylamino)cyclobutyl)acetate (1.2 g, 4.7 mmol) and hydrazine hydrate (1.4 g, 23.5 mmol) in EtOH (8 mL) was heated at 80° C. for 17 hrs. The reaction mixture was concentrated and the residue was dissolved in DCM (20 mL). The organic phase was washed with saturated sodium chloride (10 mL) and water (10 mL). The water layer was exacted with EtOAc (3×). The combined organic layer was dried over Na2SO4 and concentrated to afford tert-butyl 3-(2-hydrazinyl-2-oxoethyl)cyclobutylcarbamate (1.1 g, 97%). ESI-MS (EI+, m/z): 244 [M+H]+.

後処理

  1. concentrationThe reaction mixture was concentrated
  2. dissolutionthe residue was dissolved in DCM (20 mL)
  3. washThe organic phase was washed with saturated sodium chloride (10 mL) and water (10 mL)
  4. dry with materialThe combined organic layer was dried over Na2SO4
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-2a42f8e28bc84e5ca15b7903eafe4619
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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