Trifluoroacetic acid → HCID 18506779、化合物

HRID 1355361ノート

反応式

HRID 1355361 の反応式
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

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 10112177HCID 10112177、化合物

生成物 1

HCID 18506779HCID 18506779、化合物収率 47%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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)+.

後処理

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

出典と根拠

ORDレコード
ord-be00d7fac28e4bf39be206a4b4e2e971
出典データセット
uspto-grants-2003_07
特許番号
US06586422B2

反応ノート

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