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

HRID 604490ノート

反応式

HRID 604490 の反応式
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

参加物

6

反応物 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

生成物 1

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

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 57417360Sodium chloride; water溶媒

実験手順

[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%.

後処理

  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

出典と根拠

ORDレコード
ord-dfbcf9733a9c4367b58c1bd176115307
出典データセット
uspto-grants-2011_03
特許番号
US07910613B2

反応ノート

読み込み中…