Hydrochloric Acid → HCID 178437826、化合物

HRID 43978

反応式

HRID 43978 の反応式
ClCCl.[Cl:4][C:5]1[N:6]=[C:7]([C:12]([NH:14][C@H:15]2[CH2:20][CH2:19][N:18]([C:21]3[S:22][C:23]([C:27]4[N:31](CCC#N)[N:30]=[N:29][N:28]=4)=[C:24]([CH3:26])[N:25]=3)[CH2:17][C@H:16]2[O:36][CH3:37])=[O:13])[NH:8][C:9]=1[CH2:10][CH3:11].C1(C2CCCCCCCCCC=2)CCCCCCCCNN=1.Cl>C(OCC)(=O)C.O>[Cl:4][C:5]1[N:6]=[C:7]([C:12]([NH:14][C@H:15]2[CH2:20][CH2:19][N:18]([C:21]3[S:22][C:23]([C:27]4[NH:28][N:29]=[N:30][N:31]=4)=[C:24]([CH3:26])[N:25]=3)[CH2:17][C@H:16]2[O:36][CH3:37])=[O:13])[NH:8][C:9]=1[CH2:10][CH3:11]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 6344DichloromethaneHCID 536302743-(Cycloundecen-1-yl)-1,2-diazacycloundec-2-eneHCID 86648857cis(+/-)-4-Chloro-N-(1-{5-[1-(2-cyanoethyl)-1H-tetrazol-5-yl]-4-methyl-1,3-thiazol-2-yl}-3-methoxypiperidin-4-yl)-5-ethyl-1H-imidazole-2-carboxylic acid amide

生成物 1

HCID 178437826HCID 178437826、化合物収率 51.6%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8857Ethyl Acetate溶媒

実験手順

Dichloromethane (1.5 mL) was added to cis(±)-4-chloro-N-(1-{5-[1-(2-cyanoethyl)-1H-tetrazol-5-yl]-4-methyl-1,3-thiazol-2-yl}-3-methoxypiperidin-4-yl)-5-ethyl-1H-imidazole-2-carboxylic acid amide obtained in Example (262a) (16 mg, 0.03 mmol). While the mixture was stirred, diazabicycloundecene (15 mg, 0.10 mmol) was added, followed by stirring at room temperature overnight. The reaction solution was diluted with ethyl acetate and water. The organic layer was neutralized with 1 N hydrochloric acid, washed with brine, dried over anhydrous magnesium sulfate, and then concentrated under reduced pressure. The residue was solidified with diethyl ether and hexane to obtain 7 mg of the title compound as a white solid (47%).

後処理

  1. stirringby stirring at room temperature overnight
  2. washwashed with brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-dc9c4079df484dc482f8129e44f699a8
出典データセット
uspto-grants-2013_09
特許番号
US08536197B2

関連ノート

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