Hydrochloric Acid → 2-[4'-Chloro-4-(pyrrolidine-1-carbonyl)-biphen-2-yl]-quinoline-6-carboxylic acid

HRID 1788550노트

반응식

HRID 1788550 반응식
[Cl:1][C:2]1[CH:23]=[CH:22][C:5]([C:6]2[C:11]([C:12](=O)[CH3:13])=[CH:10][C:9]([C:15]([N:17]3[CH2:21][CH2:20][CH2:19][CH2:18]3)=[O:16])=[CH:8][CH:7]=2)=[CH:4][CH:3]=1.C[O:25][C:26](=[O:36])[C:27]1[CH:32]=[CH:31][C:30]([NH2:33])=[C:29]([CH:34]=O)[CH:28]=1.[OH-].[K+].Cl>CCO.O1CCOCC1>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C:6]2[C:11]([C:12]3[CH:13]=[CH:34][C:29]4[C:30](=[CH:31][CH:32]=[C:27]([C:26]([OH:25])=[O:36])[CH:28]=4)[N:33]=3)=[CH:10][C:9]([C:15]([N:17]3[CH2:18][CH2:19][CH2:20][CH2:21]3)=[O:16])=[CH:8][CH:7]=2)=[CH:22][CH:23]=1

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 14797Potassium HydroxideHCID 46911801Methyl 4-amino-3-formylbenzoateHCID 860272831-[4'-Chloro-4-(pyrrolidine-1-carbonyl)-biphen-2-yl]-ethanone

생성물 1

HCID 576029872-[4'-Chloro-4-(pyrrolidine-1-carbonyl)-biphen-2-yl]-quinoline-6-carboxylic acid

시약·촉매·용매 2

HCID 702Ethanol용매2회HCID 312751,4-Dioxane용매

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온도
75 °C

실험 절차

To a mixture of Compound 259a (0.388 g, 1.184 mmol) and Compound 7 (0.223 g, 1.243 mmol) was added a solution of KOH (0.234 g, 3.55 mmol) in EtOH (18 mL). The reaction mixture was stirred under Ar at 75° C. for 16 h. EtOH (10 mL) was added to make a clean solution, which was neutralized by adding 4 N HCl in dioxane (about 1 mL) to pH 3. After evaporation of solvent, H2O (15 mL) was added and the precipitates were collected by filtration, washed with water and dried. Yield 0.125 g, 89%. MS: 457.12, 458.13 (M+H+).

후처리

  1. customAfter evaporation of solvent, H2O (15 mL)
  2. additionwas added
  3. filtrationthe precipitates were collected by filtration
  4. washwashed with water
  5. customdried

출처 및 근거

ORD 기록
ord-fc0595cebb4e4adfa1177ca50db6b467
출처 데이터셋
uspto-grants-2009_03
특허 번호
US07511145B2

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