Toluene-4-thiosulfonic acid S-(4,5-bis-tert-butoxycarbonylamino-2-isopropyl-phenyl) ester → Toluene-4-thiosulfonic acid S-(4,5-diamino-2-isopropyl-phenyl)ester

HRID 1859565ノート

反応式

HRID 1859565 の反応式
C(OC([NH:8][C:9]1[C:14]([NH:15]C(OC(C)(C)C)=O)=[CH:13][C:12]([S:23][S:24]([C:27]2[CH:32]=[CH:31][C:30]([CH3:33])=[CH:29][CH:28]=2)(=[O:26])=[O:25])=[C:11]([CH:34]([CH3:36])[CH3:35])[CH:10]=1)=O)(C)(C)C>C(Cl)Cl>[NH2:8][C:9]1[C:14]([NH2:15])=[CH:13][C:12]([S:23][S:24]([C:27]2[CH:32]=[CH:31][C:30]([CH3:33])=[CH:29][CH:28]=2)(=[O:26])=[O:25])=[C:11]([CH:34]([CH3:36])[CH3:35])[CH:10]=1

参加物

3

反応物 1

HCID 69753768Toluene-4-thiosulfonic acid S-(4,5-bis-tert-butoxycarbonylamino-2-isopropyl-phenyl) ester

生成物 1

HCID 69734761Toluene-4-thiosulfonic acid S-(4,5-diamino-2-isopropyl-phenyl)ester

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Toluene-4-thiosulfonic acid S-(4,5-bis-tert-butoxycarbonylamino-2-isopropyl-phenyl)ester (prepared in Example UU-1; 8.88 g, 16.6 mmol) was dissolved in CH2Cl2 (25 mL), and HCl gas was bubbled through the solution for 15 minutes. The reaction mixture was stirred at room temperature for 90 minutes. The solvents were evaporated, and the residue was dissolved in MeOH (10 mL) and treated with pH 7.5 buffer. The precipitate that formed was filtered and dried. MS(APCI): 337 (M+H).

後処理

  1. customHCl gas was bubbled through the solution for 15 minutes
  2. customThe solvents were evaporated
  3. dissolutionthe residue was dissolved in MeOH (10 mL)
  4. additiontreated with pH 7.5 buffer
  5. customThe precipitate that formed
  6. filtrationwas filtered
  7. customdried

出典と根拠

ORDレコード
ord-b566c186dab641468afa6d3823c932d2
出典データセット
uspto-grants-2003_03
特許番号
US06528510B1

反応ノート

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