2-Methoxyethylamine → HCID 59353095, 화합물

HRID 1914704노트

반응식

HRID 1914704 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:9]=[C:10]([N+:12]([O-:14])=[O:13])[CH:11]=1)[C:6]([OH:8])=O.Cl.CN(C)CCCN=C=NCC.[CH3:27][O:28][CH2:29][CH2:30][NH2:31]>C(Cl)Cl>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:9]=[C:10]([N+:12]([O-:14])=[O:13])[CH:11]=1)[C:6]([NH:31][CH2:30][CH2:29][O:28][CH3:27])=[O:8]

참가 물질

5

반응물 3

HCID 80182-MethoxyethylamineHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 53002123-Methoxy-5-nitrobenzoic acid

생성물 1

HCID 59353095HCID 59353095, 화합물수율 100.3%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 3-methoxy-5-nitrobenzoic acid (1 g; 5.1 mmol; 1 eq) DCM (40 mL) is added N-(3-dimethylaminopropyl)-N′-ethylcarbodiimide hydrochloride (972 mg; 5.1 mmol; 1 eq). After 5 min, 2-methoxyethylamine (381 mg; 5.1 mmol; 1 eq) is added and the reaction mixture is stirred at room temperature for 2 h. The reaction mixture is then quenched with water and the expected product extracted with EtOAc. The organic phase is washed with an aqueous solution of Na2CO3 then dried over MgSO4. The solvent is evaporated to dryness to afford (1.3 g (100%) of the title compound as an orange oil. HPLC (max plot) 73.0%; Rt 2.98 min.

후처리

  1. customThe reaction mixture is then quenched with water
  2. extractionthe expected product extracted with EtOAc
  3. washThe organic phase is washed with an aqueous solution of Na2CO3
  4. dry with materialthen dried over MgSO4
  5. customThe solvent is evaporated to dryness

출처 및 근거

ORD 기록
ord-c35e383d89f54b798ee602e7be7172ab
출처 데이터셋
uspto-grants-2013_12
특허 번호
US08614215B2

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