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

HRID 38258

반응식

HRID 38258 반응식
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]

참가 물질

8

반응물 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

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-78899de241734231a9ed10a9819cd875
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08524715B2

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