Hydrochloric Acid → HCID 178447286、化合物

HRID 1739089ノート

反応式

HRID 1739089 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]([CH2:26][C:27]([CH2:35][CH3:36])([CH2:33][CH3:34])[C:28]([O:30]CC)=[O:29])[C:20](=[O:25])[CH2:21][CH2:22][CH2:23][CH3:24])=[CH:14][CH:13]=2)=[N:4][N:3]=[N:2]1.[OH-].[Na+].Cl.C(Cl)Cl.CO>C(O)C>[CH2:33]([C:27]([CH2:26][N:19]([CH2:18][C:15]1[CH:14]=[CH:13][C:12]([C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=2[C:5]2[NH:4][N:3]=[N:2][N:1]=2)=[CH:17][CH:16]=1)[C:20](=[O:25])[CH2:21][CH2:22][CH2:23][CH3:24])([CH2:35][CH3:36])[C:28]([OH:30])=[O:29])[CH3:34]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 21226129Dichloromethane methanolHCID 178447287HCID 178447287、化合物

生成物 1

HCID 178447286HCID 178447286、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

1.146 g of ethyl N-[(2'-(1H-tetrazol-5-yl)biphenyl-4-yl)methyl]-N-valeryl-2-aminomethyl-2-ethylbutyrate are dissolved in 10 ml of ethanol, treated with 4.66 ml of 2N NaOH solution and heated to reflux for 20 hours. After cooling to room temperature and addition of 4.66 ml of 2N hydrochloric acid, the mixture is evaporated. The product is isolated by chromatography on silica gel 60 (40-63 μm) using CH2Cl2 --MeOH 80:20, Rf =0.38 (system N8). MS (FAB): m /e 486 (M+ +Na), 502 (M+ +K).

後処理

  1. temperatureheated
  2. temperatureto reflux for 20 hours
  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-6778ea5bb6144a3c90b3da25f2e60cb6
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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