Trifluoroacetic acid → Molidustat

HRID 242277노트

반응식

HRID 242277 반응식
C(O[C:4](=[O:15])[C:5]([N:10]1[CH:14]=[CH:13][N:12]=[N:11]1)=[CH:6][N:7](C)C)C.[NH:16]([C:18]1[N:23]=[CH:22][N:21]=[C:20]([N:24]2[CH2:29][CH2:28][O:27][CH2:26][CH2:25]2)[CH:19]=1)N.C(O)(C(F)(F)F)=O>C(OCC)(=O)C>[N:24]1([C:20]2[N:21]=[CH:22][N:23]=[C:18]([N:16]3[C:4](=[O:15])[C:5]([N:10]4[CH:14]=[CH:13][N:12]=[N:11]4)=[CH:6][NH:7]3)[CH:19]=2)[CH2:25][CH2:26][O:27][CH2:28][CH2:29]1

참가 물질

5

반응물 3

HCID 6422Trifluoroacetic acidHCID 13393622(6-Morpholin-4-ylpyrimidin-4-yl)hydrazineHCID 66726233Ethyl 3-(dimethylamino)-2-(1H-1,2,3-triazol-1-yl)acrylate

생성물 1

HCID 59603622Molidustat수율 61.5%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

반응 조건

온도
5 °C

실험 절차

1.9 g (8.8 mmol) of the compound from Example 3A and 1.9 g (9.7 mmol) of the compound from Example 16A are initially introduced into 25 ml ethyl acetate and 504 mg (4.4 mmol) TFA are added at RT. The mixture is stirred under reflux for 16 h, then cooled to 5° C. and subsequently stirred for a further 2 h. The solid formed is filtered off, washed with ethyl acetate and dried first in air and thereafter under a high vacuum. 1.7 g of product are obtained.

후처리

  1. additionare added at RT
  2. temperatureunder reflux for 16 h
  3. stirringsubsequently stirred for a further 2 h
  4. customThe solid formed
  5. filtrationis filtered off
  6. washwashed with ethyl acetate
  7. customdried first in air

출처 및 근거

ORD 기록
ord-51f392fa7b914261b19b7a78822ad7c1
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08653111B2

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