Hydrochloric Acid → HCID 178447284、化合物

HRID 1739080ノート

反応式

HRID 1739080 の反応式
[NH:1]1[C:5]([C:6]2[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=2[C:12]2[CH:17]=[CH:16][C:15]([CH2:18][N:19]([C:29](=O)[CH2:30][CH2:31][CH2:32][CH3:33])[C:20]3(C([O-])=O)[CH2:24][CH2:23][CH2:22][CH:21]3[CH3:25])=[CH:14][CH:13]=2)=[N:4][N:3]=[N:2]1.[OH-:35].[Na+].Cl.C(Cl)Cl.[CH3:41][OH:42].C([OH:45])C>>[NH:1]1[C:5]([C:6]2[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=2[C:12]2[CH:13]=[CH:14][C:15]([CH2:18][N:19]([CH2:20][C:24]3([C:41]([OH:45])=[O:42])[CH2:25][CH2:21][CH2:22][CH2:23]3)[C:29](=[O:35])[CH2:30][CH2:31][CH2:32][CH3:33])=[CH:16][CH:17]=2)=[N:4][N:3]=[N:2]1

参加物

6

反応物 5

HCID 313Hydrochloric AcidHCID 702EthanolHCID 14798Sodium HydroxideHCID 21226129Dichloromethane methanolHCID 178447282HCID 178447282、化合物

生成物 1

HCID 178447284HCID 178447284、化合物

実験手順

0.979 g of N-[(2'-(1H-tetrazol-5-yl)biphenyl-4-yl)methyl]-N-valeryl-1-amino-methylcyclopentane-1-carboxylate are dissolved in 10 ml of ethanol and treated with 4 ml of 2N NaOH solution, and the mixture is heated to reflux for 23 h. After cooling to room temperature and adding 4.5 ml of 2N hydrochloric acid, the mixture is evaporated and the product is isolated by chromatography on silica gel 60 (40-63 μm) using CH2Cl2 --MeOH 95:5, Rf =0.35 (system N8). MS (FAB): m/e 462 (M+ +H).

後処理

  1. temperaturethe mixture is heated
  2. temperatureto reflux for 23 h
  3. customthe mixture is evaporated
  4. customthe product is isolated by chromatography on silica gel 60 (40-63 μm)

出典と根拠

ORDレコード
ord-901f824275714f8087597d3fa7f5e077
出典データセット
uspto-grants-1999_10
特許番号
US05965592

反応ノート

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