Diethyl 2-acetylglutarate → HCID 136067006, 화합물

HRID 129007

반응식

HRID 129007 반응식
CC[O-].[Na+].Cl.[CH3:6][O:7][CH2:8][C:9]([NH2:11])=[NH:10].[C:12]([CH:15]([CH2:21][CH2:22][C:23]([O:25][CH2:26][CH3:27])=[O:24])[C:16](OCC)=[O:17])(=O)[CH3:13]>CCO>[CH3:13][C:12]1[N:11]=[C:9]([CH2:8][O:7][CH3:6])[NH:10][C:16](=[O:17])[C:15]=1[CH2:21][CH2:22][C:23]([O:25][CH2:26][CH3:27])=[O:24]

참가 물질

5

반응물 3

HCID 73915Diethyl 2-acetylglutarateHCID 2723922Sodium ethoxideHCID 135486022-Methoxyethanimidamide hydrochloride

생성물 1

HCID 136067006HCID 136067006, 화합물수율 42%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of NaOEt (0.088 mol) in EtOH (prepared from 2.0 g of Na and 70 mL of EtOH), methoxyacetamidine hydrochloride (5.4 g, 0.044 mol), and diethyl acetylglutarate (10.0 g, 0.044 mol) was heated under reflux for 24 h. The mixture was concentrated, taken up in water, acidified to pH 4 with conc. HCl, and extracted with CH2Cl2. The extracts were washed with brine, dried (MgSO4), and concentrated. Trituration with ether gave 4.6 g (42%) of product as an off-white solid, mp 87°-90° C.

후처리

  1. temperaturewas heated
  2. temperatureunder reflux for 24 h
  3. concentrationThe mixture was concentrated
  4. extractionextracted with CH2Cl2
  5. washThe extracts were washed with brine
  6. dry with materialdried (MgSO4)
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-2e0daf3a169947c4b577469e4a661227
출처 데이터셋
uspto-grants-1995_11
특허 번호
US05466692

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