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 23491ノート

反応式

HRID 23491 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-5fa63e22d0ae4f559d38c467eb838e0c
出典データセット
uspto-grants-2005_02
特許番号
US06852711B2

反応ノート

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