Acetic Acid → 3-Oxo-2,3,4,4a, 5,6,8,9-octahydro-1,2,7-triaza-benzocycloheptene-7-carboxylic acid tert-butyl ester

HRID 400456노트

반응식

HRID 400456 반응식
C(O)(=O)C.[C:5]([O:9][C:10]([N:12]1[CH2:18][CH2:17][C:16](=O)[CH:15]([CH2:20][C:21]([OH:23])=O)[CH2:14][CH2:13]1)=[O:11])([CH3:8])([CH3:7])[CH3:6].O.[NH2:25][NH2:26]>C1COCC1>[C:5]([O:9][C:10]([N:12]1[CH2:18][CH2:17][C:16]2=[N:25][NH:26][C:21](=[O:23])[CH2:20][CH:15]2[CH2:14][CH2:13]1)=[O:11])([CH3:8])([CH3:7])[CH3:6]

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 24654Hydrazine hydrate (1:1)HCID 834890002-(1-Tert-butoxycarbonyl-5-oxo-azepan-4-YL)acetic acid

생성물 1

HCID 866865123-Oxo-2,3,4,4a, 5,6,8,9-octahydro-1,2,7-triaza-benzocycloheptene-7-carboxylic acid tert-butyl ester

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

60 mL acetic acid was added to 16 g 4-carboxymethyl-5-oxo-azepane-1-carboxylic acid tert-butyl ester in 120 mL THF at 5° C. 14 mL hydrazine hydrate was added to the reaction and the mixture was refluxed over night. After completion of the reaction, volatiles were removed and the residue was basified with sodium carbonate and extracted with chloroform. The organic layer was dried and concentrated under reduced pressure to afford 11 g of the desired product

후처리

  1. temperaturethe mixture was refluxed over night
  2. customAfter completion of the reaction, volatiles
  3. customwere removed
  4. extractionextracted with chloroform
  5. customThe organic layer was dried
  6. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-f45dff4a0e1d4ebeb7027b0a74857ca5
출처 데이터셋
uspto-grants-2014_06
특허 번호
US08741892B2

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