Hydrochloric Acid → [2-Chloro-4-(4-fluoro-phenylamino)-phenyl]-{5-[1-(2,3-dihydroxy-propyl)-1H-[1,2,3]triazol-4-yl]-2-methyl-phenyl}-methanone

HRID 2067231노트

반응식

HRID 2067231 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([NH:8][C:9]2[CH:14]=[CH:13][C:12]([F:15])=[CH:11][CH:10]=2)[CH:5]=[CH:4][C:3]=1[C:16]([C:18]1[CH:23]=[C:22]([C:24]2[N:25]=[N:26][N:27]([CH2:29][CH:30]3[CH2:34][O:33]C(C)(C)[O:31]3)[CH:28]=2)[CH:21]=[CH:20][C:19]=1[CH3:37])=[O:17].Cl.CCOC(C)=O.O.C([O-])(O)=O.[Na+]>C1COCC1>[Cl:1][C:2]1[CH:7]=[C:6]([NH:8][C:9]2[CH:10]=[CH:11][C:12]([F:15])=[CH:13][CH:14]=2)[CH:5]=[CH:4][C:3]=1[C:16]([C:18]1[CH:23]=[C:22]([C:24]2[N:25]=[N:26][N:27]([CH2:29][CH:30]([OH:31])[CH2:34][OH:33])[CH:28]=2)[CH:21]=[CH:20][C:19]=1[CH3:37])=[O:17]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 11685044HCID 11685044, 화합물HCID 23687555EtOAc water NaHCO3

생성물 1

HCID 11705693[2-Chloro-4-(4-fluoro-phenylamino)-phenyl]-{5-[1-(2,3-dihydroxy-propyl)-1H-[1,2,3]triazol-4-yl]-2-methyl-phenyl}-methanone

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A solution of compound 123 (1.05 g, 2.02 mmol) in THF (10 mL) was added HCl (10 mL, aq., 10, 1N) and the mixture was stirred for 16 h at RT. The reaction mixture was poured into a mixture of EtOAc/water/NaHCO3. The organic phase was washed with water, brine and then dried (MgSO4), filtered and concentrated in vacuo to give the crude product. The crude product was purified by continuous gradient flash chromatography using MeOH/DCM 0:100 to 10:90 as the eluent to afford the title compound as white solid.

후처리

  1. washThe organic phase was washed with water, brine
  2. dry with materialdried (MgSO4)
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo
  5. customto give the crude product
  6. customThe crude product was purified by continuous gradient flash chromatography

출처 및 근거

ORD 기록
ord-8f208705efa74cb4a809faca34b0ea7c
출처 데이터셋
uspto-grants-2012_10
특허 번호
US08293772B2

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