Ammonia → 5-(3-Methyl-[1,2,4]oxadiazol-5-yl)-4-phenyl-thiazol-2-ylamine

HRID 604490노트

반응식

HRID 604490 반응식
C(OC(=O)[NH:7][C:8]1[S:9][C:10]([C:19]2[O:23][N:22]=[C:21]([CH3:24])[N:20]=2)=[C:11]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[N:12]=1)(C)(C)C.C(O)(C(F)(F)F)=O.N>C(O)(=O)C.[Cl-].[Na+].O>[CH3:24][C:21]1[N:20]=[C:19]([C:10]2[S:9][C:8]([NH2:7])=[N:12][C:11]=2[C:13]2[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=2)[O:23][N:22]=1

참가 물질

6

반응물 3

HCID 222AmmoniaHCID 6422Trifluoroacetic acidHCID 57709599[5-(3-Methyl-[1,2,4]oxadiazol-5-yl)-4-phenyl-thiazol-2-yl]-carbamic Acid tert-butyl ester

생성물 1

HCID 577095965-(3-Methyl-[1,2,4]oxadiazol-5-yl)-4-phenyl-thiazol-2-ylamine수율 98%

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 57417360Sodium chloride; water용매

실험 절차

[5-(3-Methyl-[1,2,4]oxadiazol-5-yl)-4-phenyl-thiazol-2-yl]-carbamic acid tert-butyl ester was suspended in glacial acetic acid (20 mL). TFA (20 mL) was added. The reaction mixture was stirred at room temperature overnight. The reaction mixture was added to brine (100 mL) and pH was adjusted to pH 10 with ammonia. The mixture was extracted with EtOAc (2×75 mL). The combined organic phases was washed with brine (50 mL), dried with MgSO4 and solvents were removed in vacuo to give a white solid. Yield 98%.

후처리

  1. extractionThe mixture was extracted with EtOAc (2×75 mL)
  2. washThe combined organic phases was washed with brine (50 mL)
  3. dry with materialdried with MgSO4 and solvents
  4. customwere removed in vacuo
  5. customto give a white solid

출처 및 근거

ORD 기록
ord-dfbcf9733a9c4367b58c1bd176115307
출처 데이터셋
uspto-grants-2011_03
특허 번호
US07910613B2

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