Hydrochloric Acid → HCID 68580003、化合物

HRID 2234022ノート

反応式

HRID 2234022 の反応式
O.[OH-].[Na+].[Cl:4][C:5]1[C:9]([Cl:10])=[C:8]([CH3:11])[NH:7][C:6]=1[C:12]([NH:14][CH:15]1[CH2:20][CH2:19][N:18]([C:21]2[C:30]3[C:25](=[CH:26][CH:27]=[CH:28][CH:29]=3)[CH:24]=[C:23]([C:31]([O:33]C)=[O:32])[N:22]=2)[CH2:17][CH2:16]1)=[O:13].Cl>C1COCC1.CCOC(C)=O>[Cl:4][C:5]1[C:9]([Cl:10])=[C:8]([CH3:11])[NH:7][C:6]=1[C:12]([NH:14][CH:15]1[CH2:16][CH2:17][N:18]([C:21]2[C:30]3[C:25](=[CH:26][CH:27]=[CH:28][CH:29]=3)[CH:24]=[C:23]([C:31]([OH:33])=[O:32])[N:22]=2)[CH2:19][CH2:20]1)=[O:13]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 14798Sodium HydroxideHCID 68579750methyl 1-(4-{[(3,4-dichloro-5-methyl-1H-pyrrol-2-yl)carbonyl]amino}piperidin-1-yl)isoquinoline-3-carboxylate

生成物 1

HCID 68580003HCID 68580003、化合物収率 73.7%

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒HCID 8857Ethyl Acetate溶媒2 回

反応条件

温度
80 °C

実験手順

In a mixture of 20 ml THF, 5 ml H2O, and 1 ml 50 wt % NaOH (aq) was dissolved methyl 1-(4-{[(3,4-dichloro-5-methyl-1H-pyrrol-2-yl)carbonyl]amino}piperidin-1-yl)isoquinoline-3-carboxylate (Example 301; 70 mg). The solution was stirred at 80° C. for 1 hr. The solution was cooled to room temperature, diluted with EtOAc and acidified with dilute HCl (aq). The EtOAc fraction was isolated, at which time a white solid precipitated from solution. The solid was collected by filtration and washed with acetonitrile to yield 50 mg white solid product.

後処理

  1. temperatureThe solution was cooled to room temperature
  2. customprecipitated from solution
  3. filtrationThe solid was collected by filtration
  4. washwashed with acetonitrile

出典と根拠

ORDレコード
ord-459a067e62e14c9baed96479d30ec4dc
出典データセット
uspto-grants-2010_05
特許番号
US07709503B2

反応ノート

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