Sodium Chloride → HCID 178512574、化合物

HRID 56600

反応式

HRID 56600 の反応式
C([N:4](CC)C(C)C)(C)C.O.NN.Cl.[N+:14]([C:17]1[CH:22]=[CH:21][C:20]([C:23](=[NH:25])[NH2:24])=[CH:19][CH:18]=1)([O-:16])=[O:15].[Cl-].[Na+]>CO.C(OCC)(=O)C>[N+:14]([C:17]1[CH:18]=[CH:19][C:20]([C:23](=[NH:24])[NH:25][NH2:4])=[CH:21][CH:22]=1)([O-:16])=[O:15]

参加物

7

反応物 4

HCID 5234Sodium ChlorideHCID 24654Hydrazine hydrate (1:1)HCID 81531DiisopropylethylamineHCID 1706254-Nitrobenzamidine hydrochloride

生成物 1

HCID 178512574HCID 178512574、化合物

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8857Ethyl Acetate溶媒

実験手順

At 0° C., 5.2 ml (29.8 mmol, 3 eq.) of N,N-diisopropylethylamine and 0.62 g (purity 80%, 9.92 mmol, 1.0 eq.) of hydrazine monohydrate were added to a solution of 2.0 g (9.92 mmol) of 4-nitrobenzenecarboximidamide monohydrochloride in 20 ml of methanol, and the mixture was stirred at RT for 64 h. The reaction mixture was then added to 10% strength sodium chloride solution and, after addition of ethyl acetate and phase separation, was extracted twice with ethyl acetate. The combined organic phases were dried over sodium sulphate, filtered and concentrated under reduced pressure. Yield: 1.7 g (93% of theory)

後処理

  1. extractionwas extracted twice with ethyl acetate
  2. dry with materialThe combined organic phases were dried over sodium sulphate
  3. filtrationfiltered
  4. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-05d02b578f3241d1adb7583028d7eb0a
出典データセット
uspto-grants-2016_09
特許番号
US09434690B2

関連ノート

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