Hydrochloric Acid → HCID 68580003, 화합물

HRID 2234022노트

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HRID 2234022 반응식
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]

참가 물질

7

반응물 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

생성물 1

HCID 68580003HCID 68580003, 화합물수율 73.7%

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매HCID 8857Ethyl Acetate용매2회

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온도
80 °C

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-459a067e62e14c9baed96479d30ec4dc
출처 데이터셋
uspto-grants-2010_05
특허 번호
US07709503B2

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