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Hydrochloric Acid → HCID 54437783, 화합물

HRID 1374985
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HRID 1374985 반응식
[CH2:1]([NH2:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(=O)([O-])[O-].[K+].[K+].[CH3:15][O:16][C:17](=[O:34])[C@H:18]([NH:29][C:30](=[O:33])[CH2:31]Cl)[CH2:19][C:20]1[CH:25]=[CH:24][C:23]([CH3:26])=[C:22]([O:27][CH3:28])[CH:21]=1.Cl>CN(C)C=O.ClCCl>[CH3:15][O:16][C:17](=[O:34])[C@H:18]([NH:29][C:30](=[O:33])[CH2:31][NH:8][CH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1)[CH2:19][C:20]1[CH:25]=[CH:24][C:23]([CH3:26])=[C:22]([O:27][CH3:28])[CH:21]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 7504BenzylamineHCID 11430Potassium CarbonateHCID 54076724HCID 54076724, 화합물

생성물 1

HCID 54437783HCID 54437783, 화합물

시약·촉매·용매 2

HCID 6228Dimethylformamide용매
HCID 6344
Dichloromethane
용매

반응 조건

온도
35 °C

실험 절차

Benzylamine (1.65 g) and potassium carbonate (1.28 g) were added successively to a solution of (2R)-2-[N-(chloroacetyl)amino]-3-(3-methoxy-4-methylphenyl)propionic acid methyl ester (1.85 g) in N,N-dimethylformamide (15 ml) at 20° C. After being stirred at 35° C. for 1.5 hours, the mixture was poured into a mixture of ice-water (20 ml) and dichloromethane (20 ml). After the mixture was adjusted to pH 9 with diluted aqueous hydrochloric acid under stirring, the organic layer was separated, washed with brine (20 ml), dried over magnesium sulfate and evaporated under reduced pressure to give an oil of (2R)-2-[N-(benzylaminoacetyl)-amino]-3-(3-methoxy-4-methylphenyl)propionic acid methyl ester. A solution of (2R)-2-[N-(benzylaminoacetyl)amino]-3-(3-methoxy-4-methylphenyl)propionic acid methyl ester obtained by above procedure and acetic acid (0.18 ml) in isopropyl alcohol (10 ml) was stirred for 12 hours under reflux.

후처리

  1. stirringunder stirring
  2. customthe organic layer was separated
  3. washwashed with brine (20 ml)
  4. dry with materialdried over magnesium sulfate
  5. customevaporated under reduced pressure

출처 및 근거

ORD 기록
ord-2780cb9309fa430c996dc542320aff99
출처 데이터셋
uspto-grants-2007_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07166598B2

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