Trifluoroacetic acid → HCID 18506779, 화합물

HRID 1355361노트

반응식

HRID 1355361 반응식
C(OC(=O)[NH:7][CH2:8][CH2:9][NH:10][C:11]1[N:12]=[N:13][C:14]([C:28]#[N:29])=[C:15]([N:17]2[CH2:23][CH2:22][C:21]3[CH:24]=[CH:25][CH:26]=[CH:27][C:20]=3[CH2:19][CH2:18]2)[N:16]=1)(C)(C)C.[F:31][C:32]([F:37])([F:36])[C:33]([OH:35])=[O:34]>ClCCl>[F:31][C:32]([F:37])([F:36])[C:33]([OH:35])=[O:34].[NH2:7][CH2:8][CH2:9][NH:10][C:11]1[N:12]=[N:13][C:14]([C:28]#[N:29])=[C:15]([N:17]2[CH2:23][CH2:22][C:21]3[CH:24]=[CH:25][CH:26]=[CH:27][C:20]=3[CH2:19][CH2:18]2)[N:16]=1

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 10112177HCID 10112177, 화합물

생성물 1

HCID 18506779HCID 18506779, 화합물수율 47%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 60 mg (0.15 mmol) of {2-[6-cyano-5-(1,2,4,5-tetrahydro-benzo[d]azepin-3-yl)-[1,2,4]triazin-3-ylamino]-ethyl}-carbamic acid tert-butyl ester as prepared in example 8 in 2 ml of dichloromethane were added 0.2 ml of trifluoroacetic acid. The reaction mixture was stirred at room temperature for one hour and then evaporated under reduced pressure. The solid residue was dispersed in ether. The resulting solid was filtered and gave 30 mg (47% of theory) of 3-(2-amino-ethylamino)-5 -(1,2,4,5-tetrahydro-benzo[d]azepin-3-yl)-[1,2,4]triazine-6-carbonitrile trifluoro-acetate as an off-white solid; MS: 310 (M+H)+.

후처리

  1. customevaporated under reduced pressure
  2. additionThe solid residue was dispersed in ether
  3. filtrationThe resulting solid was filtered

출처 및 근거

ORD 기록
ord-be00d7fac28e4bf39be206a4b4e2e971
출처 데이터셋
uspto-grants-2003_07
특허 번호
US06586422B2

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