Dimethylformamide → 3,3-Diphenyl-2-(4,6-dimethyl-2-pyrimidinylamino)propionic acid

HRID 2305371노트

반응식

HRID 2305371 반응식
[NH2:1][CH:2]([CH:6]([C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1)[C:3]([OH:5])=[O:4].Cl[C:20]1[N:25]=[C:24]([CH3:26])[CH:23]=[C:22]([CH3:27])[N:21]=1.CN(C=O)C.C(=O)([O-])[O-].[Na+].[Na+]>O.C(OCC)(=O)C>[C:7]1([CH:6]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[CH:2]([NH:1][C:20]2[N:25]=[C:24]([CH3:26])[CH:23]=[C:22]([CH3:27])[N:21]=2)[C:3]([OH:5])=[O:4])[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1

참가 물질

7

반응물 4

HCID 6228DimethylformamideHCID 10340Sodium CarbonateHCID 205502-Chloro-4,6-dimethylpyrimidineHCID 2249693,3-Diphenylalanine

생성물 1

HCID 99062773,3-Diphenyl-2-(4,6-dimethyl-2-pyrimidinylamino)propionic acid수율 19.2%

시약·촉매·용매 2

HCID 962Water용매2회HCID 8857Ethyl Acetate용매

반응 조건

온도
80 °C

실험 절차

2.60 g (10.8 mmol) of 2-amino-3,3-diphenylpropionic acid and 0.64 g (4.5 mmol) of 2-chloro-4,6-dimethylpyrimidine were introduced into a mixture of 16 ml of DMF and 16 ml of water, 0.57 g (5.4 mmol) of sodium carbonate was added and the mixture was stirred at 80° C. for 24 hours. Then 100 ml of ethyl acetate and a little water were added, and the phases were separated. The aqueous phase was acidified (pH 1-2) with 6 normal hydrochloric acid. The resulting precipitate was filtered off with suction and washed with ethyl acetate, then dried. 0.30 g (19.2%) of a white powder of melting point 172-174° C. was obtained.

후처리

  1. additionwas added
  2. customthe phases were separated
  3. filtrationThe resulting precipitate was filtered off with suction
  4. washwashed with ethyl acetate
  5. customdried

출처 및 근거

ORD 기록
ord-ebd08b2edc0845e9b5cfa326e9b2da3a
출처 데이터셋
uspto-grants-2002_08
특허 번호
US06440975B1

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