Trifluoroacetic acid → (R)-N5-[amino (nitroimino)-methyl]-N-[2-(4-hydroxyphenyl) ethyl]-ornithinamide trifluoroacetate

HRID 2393643노트

반응식

HRID 2393643 반응식
[NH2:1][C:2](=[N:28][N+:29]([O-:31])=[O:30])[NH:3][CH2:4][CH2:5][CH2:6][C@H:7]([C:16]([NH:18][CH2:19][CH2:20][C:21]1[CH:26]=[CH:25][C:24]([OH:27])=[CH:23][CH:22]=1)=[O:17])[NH:8]C(OC(C)(C)C)=O.[F:32][C:33]([F:38])([F:37])[C:34]([OH:36])=[O:35]>ClCCl>[NH2:1][C:2](=[N:28][N+:29]([O-:31])=[O:30])[NH:3][CH2:4][CH2:5][CH2:6][C@H:7]([C:16]([NH:18][CH2:19][CH2:20][C:21]1[CH:22]=[CH:23][C:24]([OH:27])=[CH:25][CH:26]=1)=[O:17])[NH2:8].[F:32][C:33]([F:38])([F:37])[C:34]([O-:36])=[O:35]

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 136381088HCID 136381088, 화합물

생성물 1

HCID 136381086(R)-N5-[amino (nitroimino)-methyl]-N-[2-(4-hydroxyphenyl) ethyl]-ornithinamide trifluoroacetate

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 0.8 g (1.82 mMol) of (R)-N5 -[amino(nitroimino)methyl]-N2 -(tert.-butoxycarbonyl)-N-[2-(4-hydroxyphenyl)ethyl]-ornithinamide in 20 ml of dichloromethane, externally cooled with crushed ice/ethanol, were added 2.5 ml of trifluoroacetic acid, then the mixture was allowed to come up to ambient temperature and stirred for a further 4 hours at this temperature. The clear solution obtained was evaporated down in a water jet vacuum and combined twice with 10 ml of water and once with 10 ml of toluene and then dried once more. The amorphous (R)-N5 -[amino(nitroimino)-methyl]-N-[2-(4-hydroxyphenyl)ethyl]-ornithinamide-trifluoroacetate obtained (0.61 g, 74% of theory), Rf 0.33 (test conditions as in Example 5d) was further processed without any more purification.

후처리

  1. customto come up to ambient temperature
  2. customThe clear solution obtained
  3. customwas evaporated down in a water jet vacuum
  4. customdried once more

출처 및 근거

ORD 기록
ord-ec00cf9357224717a333222a1fd526f4
출처 데이터셋
uspto-grants-1998_09
특허 번호
US05807875

반응 노트

불러오는 중…