Ethyl 2-formylbutanoate → HCID 178457579、化合物

HRID 1253164

反応式

HRID 1253164 の反応式
Cl.[CH2:2]([N:5]=[C:6]([NH2:21])[NH:7][C:8]1[CH:13]=[CH:12][N:11]=[C:10]([CH2:14][CH2:15][CH2:16][CH2:17][C:18]([NH2:20])=[NH:19])[N:9]=1)[CH2:3][CH3:4].[Na].[CH:23]([CH:25]([CH2:31][CH3:32])[C:26](OCC)=O)=[O:24]>CO>[CH2:2]([N:5]=[C:6]([NH2:21])[NH:7][C:8]1[CH:13]=[CH:12][N:11]=[C:10]([CH2:14][CH2:15][CH2:16][CH2:17][C:18]2[N:20]=[C:23]([OH:24])[C:25]([CH2:31][CH3:32])=[CH:26][N:19]=2)[N:9]=1)[CH2:3][CH3:4]

参加物

5

反応物 3

HCID 289299Ethyl 2-formylbutanoateHCID 5360545SodiumHCID 201371495-(4-[2-Propylguanidino]pyrimid-2-yl)valeramidine hydrochloride

生成物 1

HCID 178457579HCID 178457579、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A mixture of 5-(4-[2-propylguanidino]pyrimid-2-yl)valeramidine hydrochloride (0.4 g.) and the sodium salt of ethyl 2-formylbutyrate (1.5 g.) in MeOH (5 ml.) was heated under reflux for 4 hours. The solvent was evaporated in vacuo and the residue was partitioned between water (pH 7) and EtOAc. The EtOAc layer was separated, dried (MgSO4) and evaporated in vacuo to give 2-[4-(4-(2-propylguanidino]pyrimid-2-yl)butyl]-5-ethyl-4-hydroxypyrimidine as an oil (0.13 g.) which was characterised by conversion to the bis hydrogen maleate salt (0.11 g.), m.p. 140°-142°.

後処理

  1. temperatureunder reflux for 4 hours
  2. customThe solvent was evaporated in vacuo
  3. customthe residue was partitioned between water (pH 7) and EtOAc
  4. customThe EtOAc layer was separated
  5. dry with materialdried (MgSO4)
  6. customevaporated in vacuo

出典と根拠

ORDレコード
ord-6d6b062b552241ad9e238f1746723804
出典データセット
uspto-grants-1988_05
特許番号
US04748165

関連ノート

読み込み中…