1,2-Dichloroethane → HCID 178454346、化合物

HRID 1875182ノート

反応式

HRID 1875182 の反応式
[NH2:1][CH2:2][C:3]1[C:4]([F:22])=[C:5]([O:10][C:11]2[CH:12]=[C:13]([CH:16]=[C:17]([CH:19]3[CH2:21][CH2:20]3)[CH:18]=2)[C:14]#[N:15])[C:6]([Cl:9])=[CH:7][CH:8]=1.[CH3:23][C:24]([O:27][C:28]([N:30]([C:40]([O:42][C:43]([CH3:46])([CH3:45])[CH3:44])=[O:41])[C:31]1[NH:32][C:33]([C:37](O)=[O:38])=[C:34]([Cl:36])[N:35]=1)=[O:29])([CH3:26])[CH3:25].C1C=CC2N(O)N=NC=2C=1.C(Cl)CCl>CN(C=O)C.CCOC(C)=O>[CH3:46][C:43]([O:42][C:40]([N:30]([C:31]1[NH:32][C:33]([C:37]([NH:1][CH2:2][C:3]2[CH:8]=[CH:7][C:6]([Cl:9])=[C:5]([O:10][C:11]3[CH:18]=[C:17]([CH:19]4[CH2:20][CH2:21]4)[CH:16]=[C:13]([C:14]#[N:15])[CH:12]=3)[C:4]=2[F:22])=[O:38])=[C:34]([Cl:36])[N:35]=1)[C:28]([O:27][C:24]([CH3:23])([CH3:25])[CH3:26])=[O:29])=[O:41])([CH3:44])[CH3:45]

参加物

7

反応物 4

HCID 111,2-DichloroethaneHCID 757711-HydroxybenzotriazoleHCID 68487554HCID 68487554、化合物HCID 178454348HCID 178454348、化合物

生成物 1

HCID 178454346HCID 178454346、化合物収率 84%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of 3-{[3-(aminomethyl)-6-chloro-2-fluorophenyl]oxy}-5-cyclopropylbenzonitrile (95 mg, 0.299 mmol), 2-(bis{[(1,1-dimethylethyl)oxy]carbonyl}amino)-4-chloro-1H-imidazole-5-carboxylic acid (120 mg, 0.299 mmol) and HOBT (45.7 mg, 0.299 mmol) in DMF (3 ml) was added EDC (57.2 mg, 0.299 mmol) and the reaction mixture was stirred at RT for 45 minutes. The reaction mixture was diluted with EtOAc and washed with water. The solvent was removed and the crude material bis(1,1-dimethylethyl)(4-chloro-5-{[({4-chloro-3-[(3-cyano-5-cyclopropylphenyl)oxy]-2-fluorophenyl}methyl)amino]carbonyl}-1H-imidazol-2-yl)imidodicarbonate (165 mg, 0.250 mmol, 84% yield) was used directly in the next step. LC-MS (ES+) m/z 660 [M+H].

後処理

  1. washwashed with water
  2. customThe solvent was removed

出典と根拠

ORDレコード
ord-2679de7e8aa2410caa4a2f7f5f1b1be1
出典データセット
uspto-grants-2012_11
特許番号
US08304419B2

反応ノート

読み込み中…