Hydrochloric Acid → HCID 178487908、化合物

HRID 2112100ノート

反応式

HRID 2112100 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:9]=[CH:10][C:11]=1[N+:12]([O-:14])=[O:13])[C:6]([NH2:8])=[NH:7].Cl.C(=O)([O-])[O-].[K+].[K+].Cl[CH2:23][C:24](=O)[CH2:25][C:26]([O:28]CC)=[O:27].[I-].[K+].[OH-].[Na+]>CO.C(#N)C.O>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:6]2[NH:8][CH:23]=[C:24]([CH2:25][C:26]([OH:28])=[O:27])[N:7]=2)[CH:9]=[CH:10][C:11]=1[N+:12]([O-:14])=[O:13]

参加物

10

反応物 6

HCID 313Hydrochloric AcidHCID 4875Potassium IodideHCID 11430Potassium CarbonateHCID 14798Sodium HydroxideHCID 69484Ethyl 4-chloroacetoacetateHCID 187277063-Methoxy-4-nitrobenzimidamide

生成物 1

HCID 178487908HCID 178487908、化合物

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 962Water溶媒HCID 6342Acetonitrile溶媒

反応条件

温度
45 °C

実験手順

7 g (60% purity, 21.519 mmol) 3-methoxy-4-nitro-benzamidine are dissolved in methanol and combined with 11 ml (44 mmol) 4 N dioxanic hydrochloric acid, the solvents are eliminated in vacuo. The residue and 6.13 g (44.384 mmol) potassium carbonate are suspended in 350 ml acetonitrile and combined with 3.24 ml (22.764 mmol) ethyl 4-chloracetoacetate and 880 mg (5.301 mmol) potassium iodide. The reaction mixture is stirred for 16 h at 45° C. The reaction mixture is diluted with water and combined with 1 N sodium hydroxide solution, and extracted with ethyl acetate. The aqueous phase is adjusted to pH 1 with 1 N HCL and saturated with sodium chloride. The product is then suction filtered.

後処理

  1. extractionextracted with ethyl acetate
  2. filtrationsuction filtered

出典と根拠

ORDレコード
ord-297517bd8aa3460daf3631f0dfb8ebb8
出典データセット
uspto-grants-2009_04
特許番号
US07521457B2

反応ノート

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