Trifluoroacetic acid → Molidustat

HRID 242277ノート

反応式

HRID 242277 の反応式
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

参加物

5

反応物 3

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

生成物 1

HCID 59603622Molidustat収率 61.5%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

反応条件

温度
5 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-51f392fa7b914261b19b7a78822ad7c1
出典データセット
uspto-grants-2014_02
特許番号
US08653111B2

反応ノート

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