Hydrazine hydrate (1:1) → HCID 86701057, 화합물

HRID 1855606노트

반응식

HRID 1855606 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

HCID 86701057HCID 86701057, 화합물수율 97%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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]+.

후처리

  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

출처 및 근거

ORD 기록
ord-2a42f8e28bc84e5ca15b7903eafe4619
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08962844B2

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