Hydrochloric Acid → [3-Chloro-2-[[4-[(4-chlorophenyl)acetyl]-1-piperazinyl]-methyl]-phenoxy]-acetic Acid

HRID 38258

反応式

HRID 38258 の反応式
Cl[C:2]1[CH:12]=[CH:11][C:5]([O:6][CH2:7][C:8]([OH:10])=[O:9])=[C:4]([CH2:13][N:14]2[CH2:19][CH2:18][N:17](S(C3C=CC=CC=3)(=O)=O)[CH2:16][CH2:15]2)[CH:3]=1.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.[Cl:53][C:54]1[CH:55]=[C:56](CC(O)=O)[CH:57]=[CH:58][CH:59]=1.[OH-].[Na+].[ClH:66].C([O:70][CH2:71][CH3:72])(=O)C>CN(C=O)C>[Cl:66][C:3]1[C:4]([CH2:13][N:14]2[CH2:15][CH2:16][N:17]([C:71](=[O:70])[CH2:72][C:57]3[CH:56]=[CH:55][C:54]([Cl:53])=[CH:59][CH:58]=3)[CH2:18][CH2:19]2)=[C:5]([CH:11]=[CH:12][CH:2]=1)[O:6][CH2:7][C:8]([OH:10])=[O:9]

参加物

8

反応物 6

HCID 313Hydrochloric AcidHCID 8857Ethyl AcetateHCID 14798Sodium HydroxideHCID 158793-Chlorophenylacetic acidHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 53317503[4-chloro-2-[4-(phenylsulfonyl)-1-piperazinylmethyl]phenoxy]-acetic Acid

生成物 1

HCID 11561177[3-Chloro-2-[[4-[(4-chlorophenyl)acetyl]-1-piperazinyl]-methyl]-phenoxy]-acetic Acid

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

The product from Example 11 part (a) (300 mg) was dissolved in DMF (10 ml) and treated with HATU ((570 mg), followed by 3-chlorobenzeneacetic acid (190 mg). The reaction mixture was stirred for 18 h, treated with 1M NaOH (3 ml) and stirred for 3 h. The reaction was acidified with 2M HCl, diluted with ethyl acetate, washed with brine, dried (MgSO4) and concentrated in vacuo. The residue was purified by RPHPLC to give the title compound (110 mg).

後処理

  1. stirringstirred for 3 h
  2. washwashed with brine
  3. dry with materialdried (MgSO4)
  4. concentrationconcentrated in vacuo
  5. customThe residue was purified by RPHPLC

出典と根拠

ORDレコード
ord-78899de241734231a9ed10a9819cd875
出典データセット
uspto-grants-2013_09
特許番号
US08524715B2

関連ノート

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