Ethyl 2-formylbutanoate → HCID 178457579, 화합물

HRID 1253164

반응식

HRID 1253164 반응식
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]

참가 물질

5

반응물 3

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

생성물 1

HCID 178457579HCID 178457579, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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°.

후처리

  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

출처 및 근거

ORD 기록
ord-6d6b062b552241ad9e238f1746723804
출처 데이터셋
uspto-grants-1988_05
특허 번호
US04748165

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