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 400456ノート

反応式

HRID 400456 の反応式
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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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

後処理

  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

出典と根拠

ORDレコード
ord-f45dff4a0e1d4ebeb7027b0a74857ca5
出典データセット
uspto-grants-2014_06
特許番号
US08741892B2

反応ノート

読み込み中…