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 23491노트

반응식

HRID 23491 반응식
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

참가 물질

3

반응물 1

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-5fa63e22d0ae4f559d38c467eb838e0c
출처 데이터셋
uspto-grants-2005_02
특허 번호
US06852711B2

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