Hydrochloric Acid → HCID 178487037、化合物

HRID 1749963ノート

反応式

HRID 1749963 の反応式
[NH:1]1[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[C:3](/[CH:10]=[C:11]2\[O:12][C:13]3[C:20]([CH:21]4[CH2:26][CH2:25][N:24](C(OC(C)(C)C)=O)[CH2:23][CH2:22]4)=[C:19]([O:34][CH3:35])[CH:18]=[CH:17][C:14]=3[C:15]\2=[O:16])=[N:2]1.Cl>C(Cl)Cl.O1CCOCC1>[NH:1]1[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[C:3](/[CH:10]=[C:11]2\[O:12][C:13]3[C:20]([CH:21]4[CH2:26][CH2:25][NH:24][CH2:23][CH2:22]4)=[C:19]([O:34][CH3:35])[CH:18]=[CH:17][C:14]=3[C:15]\2=[O:16])=[N:2]1

参加物

5

反応物 2

HCID 313Hydrochloric AcidHCID 178487039HCID 178487039、化合物

生成物 1

HCID 178487037HCID 178487037、化合物収率 88.7%

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 312751,4-Dioxane溶媒

実験手順

A solution of tert-butyl (Z)-4-{2-[(1H-indazol-3-yl)methylene]-6-methoxy-3-oxo-2,3-dihydrobenzofuran-7-yl}piperidine-1-carboxylate (0.0446 g, 0.0937 mmol) in methylene chloride (3 mL) was added with a 4 M solution of hydrogen chloride in 1,4-dioxane (3 mL), and the mixture was stirred at room temperature for 2 hours. The reaction mixture was concentrated, the resulting residue was added with saturated aqueous sodium hydrogencarbonate, and the precipitated solid was collected by filtration. The solid was washed with water, and then dried under reduced pressure to obtain (Z)-2-[(1H-indazol-3-yl)methylene]-6-methoxy-7-(piperidin-4-yl)benzofuran-3(2H)-one (0.0312 g, 88%).

後処理

  1. concentrationThe reaction mixture was concentrated
  2. additionthe resulting residue was added with saturated aqueous sodium hydrogencarbonate
  3. filtrationthe precipitated solid was collected by filtration
  4. washThe solid was washed with water
  5. customdried under reduced pressure

出典と根拠

ORDレコード
ord-fe7e7c4444a44cc5bab1aec286fa4539
出典データセット
uspto-grants-2015_10
特許番号
US09156827B2

反応ノート

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