Hydrochloric Acid → 1-(4-Fluorobenzyl)-3-(3-(2-methylpyridin-4-yl)-1H-indazole-5-carboxamido)cyclohexanecarboxylic acid

HRID 530878ノート

反応式

HRID 530878 の反応式
[OH-].[Na+].O.[F:4][C:5]1[CH:40]=[CH:39][C:8]([CH2:9][C:10]2([C:35]([O:37]C)=[O:36])[CH2:15][CH2:14][CH2:13][CH:12]([NH:16][C:17]([C:19]3[CH:20]=[C:21]4[C:25](=[CH:26][CH:27]=3)[NH:24][N:23]=[C:22]4[C:28]3[CH:33]=[CH:32][N:31]=[C:30]([CH3:34])[CH:29]=3)=[O:18])[CH2:11]2)=[CH:7][CH:6]=1.Cl>CO.C1COCC1>[F:4][C:5]1[CH:40]=[CH:39][C:8]([CH2:9][C:10]2([C:35]([OH:37])=[O:36])[CH2:15][CH2:14][CH2:13][CH:12]([NH:16][C:17]([C:19]3[CH:20]=[C:21]4[C:25](=[CH:26][CH:27]=3)[NH:24][N:23]=[C:22]4[C:28]3[CH:33]=[CH:32][N:31]=[C:30]([CH3:34])[CH:29]=3)=[O:18])[CH2:11]2)=[CH:7][CH:6]=1

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 14798Sodium HydroxideHCID 67985855methyl 1-(4-fluorobenzyl)-3-(3-(2-methylpyridin-4-yl)-1H-indazole-5-carboxamido)cyclohexanecarboxylate

生成物 1

HCID 866982491-(4-Fluorobenzyl)-3-(3-(2-methylpyridin-4-yl)-1H-indazole-5-carboxamido)cyclohexanecarboxylic acid

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8028Tetrahydrofuran溶媒

反応条件

温度
70 °C

実験手順

Sodium hydroxide in water (4 M solution, 1 ml, 4 mmol) was added into a solution of methyl 1-(4-fluorobenzyl)-3-(3-(2-methylpyridin-4-yl)-1H-indazole-5-carboxamido)cyclohexanecarboxylate (0.32 mmol) in methanol (0.5 ml) and THF (2 ml). The reaction solution was stirred at 70° C. for 16 h, and 1.0 N HCl solution was added dropwise to adjust pH to 4. The resulting solution was extracted with EtOAc (10 ml, twice). The combined organic layers were dried over sodium sulfate, filtered, concentrated, and purified using HPLC to give the titled compound. LC-MS: 487.21 [M+11]. LC/MS RT=2.36 min.

後処理

  1. extractionThe resulting solution was extracted with EtOAc (10 ml
  2. dry with materialThe combined organic layers were dried over sodium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated
  5. custompurified

出典と根拠

ORDレコード
ord-7f68234ec90c4a798f79aac5422ad36c
出典データセット
uspto-grants-2016_05
特許番号
US09351965B2

反応ノート

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