Hydrochloric Acid → HCID 22727296、化合物

HRID 2086274ノート

反応式

HRID 2086274 の反応式
[Cl:1][C:2]1[CH:34]=[CH:33][C:5]2[CH:6]=[C:7]([S:10]([N:13]3[CH2:18][CH2:17][N:16]([NH:19][CH:20]4[CH2:25][CH2:24][N:23]([C:26]5[CH:31]=[CH:30][N:29]=[CH:28][CH:27]=5)[CH2:22][CH2:21]4)[C:15](=[O:32])[CH2:14]3)(=[O:12])=[O:11])[CH2:8][O:9][C:4]=2[CH:3]=1.[OH-].[Na+].Cl.[C:38](OC(=O)C)(=[O:40])[CH3:39]>C(OCC)(=O)C>[ClH:1].[Cl:1][C:2]1[CH:34]=[CH:33][C:5]2[CH:6]=[C:7]([S:10]([N:13]3[CH2:18][CH2:17][N:16]([N:19]([CH:20]4[CH2:25][CH2:24][N:23]([C:26]5[CH:31]=[CH:30][N:29]=[CH:28][CH:27]=5)[CH2:22][CH2:21]4)[C:38](=[O:40])[CH3:39])[C:15](=[O:32])[CH2:14]3)(=[O:11])=[O:12])[CH2:8][O:9][C:4]=2[CH:3]=1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 7918Acetic AnhydrideHCID 14798Sodium HydroxideHCID 9957779HCID 9957779、化合物

生成物 1

HCID 22727296HCID 22727296、化合物

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒2 回

実験手順

A solution of 4-(7-chloro-2H-benzopyran-3-sulfonyl)-1-[1-(4-pyridyl)-4-piperidinylamino]-2-piperazinone (95 mg) in acetic anhydride (4 ml) was stirred at 80° C. for 10 hours. The reaction mixture was concentrated and the residue obtained was combined with a 1N aqueous solution of sodium hydroxide and extracted with dichloromethane. The organic phase was washed with aqueous sodium bicarbonate and brine, dried and concentrated to obtain N-[(7-chloro-2H-benzopyran-3-sulfonyl)-2-oxo-1-piperazinyl]-N-[1-(4-pyridyl)-4-piperidinyllacetamide. The resultant free form was dissolved in ethyl acetate, and combined with a solution of hydrochloric acid in ethyl acetate to form a precipitate, which was collected by filtration, washed with ethyl acetate, dried under reduced pressure to obtain the title compound (90 mg) as a colorless solid.

後処理

  1. concentrationThe reaction mixture was concentrated
  2. customthe residue obtained
  3. extractionextracted with dichloromethane
  4. washThe organic phase was washed with aqueous sodium bicarbonate and brine
  5. customdried
  6. concentrationconcentrated
  7. customto obtain N-[(7-chloro-2H-benzopyran-3-sulfonyl)-2-oxo-1-piperazinyl]-N-[1-(4-pyridyl)-4-piperidinyllacetamide
  8. customto form a precipitate, which
  9. filtrationwas collected by filtration
  10. washwashed with ethyl acetate
  11. customdried under reduced pressure

出典と根拠

ORDレコード
ord-06a4b9edb41247f48c404e051adf4094
出典データセット
uspto-grants-2004_04
特許番号
US06723722B1

反応ノート

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