Hydrochloric Acid → N-[2-(2-oxo-2,3-dihydro-1H-benzimidazol-1-yl)ethyl]-acetamide

HRID 1059650ノート

反応式

HRID 1059650 の反応式
[OH-].[Na+].Cl.[NH2:4][CH2:5][CH2:6][N:7]1[C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=2[NH:9][C:8]1=[O:16].[C:17](OC(=O)C)(=[O:19])[CH3:18].Cl>O.O1CCOCC1>[O:16]=[C:8]1[N:7]([CH2:6][CH2:5][NH:4][C:17](=[O:19])[CH3:18])[C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=2[NH:9]1

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 7918Acetic AnhydrideHCID 14798Sodium HydroxideHCID 186308891-(2-aminoethyl)-2,3-dihydro-1H-1,3-benzodiazol-2-one hydrochloride

生成物 1

HCID 18630881N-[2-(2-oxo-2,3-dihydro-1H-benzimidazol-1-yl)ethyl]-acetamide

試薬・触媒・溶媒 2

HCID 962Water溶媒2 回HCID 312751,4-Dioxane溶媒

実験手順

To a cooled solution of NaOH (0.41 g, 10 mmoles) in water (5 ml) were simultaneously added 1-(2-aminoethyl)-1,3-dihydro-2H-benzimidazol-2-one hydrochloride (0.7 g, 3.3 mmoles) and a solution of acetic anhydride (0.37 ml, 3.9 mmoles) in dioxane (10 ml). The reaction mixture was stirred for 2 hours at room temperature and then taken to dryness. The residue was dissolved in water, adjusted to pH 4 with 10% aqueous HCl, and extracted with CHCl3. The organic layer was taken to dryness and from the crude residue 0.35 g of the title compound was obtained after crystallization from diethyl ether. M.p. 153° C.

後処理

  1. extractionextracted with CHCl3
  2. customwas obtained
  3. customafter crystallization from diethyl ether

出典と根拠

ORDレコード
ord-a38627d3beb243febf0f05de6de033d3
出典データセット
uspto-grants-2003_02
特許番号
US06521623B1

反応ノート

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