Hydrochloric Acid → 2,6-Diaminobenzonitrile

HRID 1076990ノート

反応式

HRID 1076990 の反応式
[N+:1]([C:4]1[CH:11]=[CH:10][CH:9]=[C:8]([N+:12]([O-])=O)[C:5]=1[C:6]#[N:7])([O-])=O.Cl.[OH-].[Na+]>O>[NH2:1][C:4]1[CH:11]=[CH:10][CH:9]=[C:8]([NH2:12])[C:5]=1[C:6]#[N:7]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 520718Dinitrobenzonitrile

生成物 1

HCID 124029832,6-Diaminobenzonitrile収率 60.2%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

2,6-Dinitrobenzonitrile (10.0 grams) is added in portions to a stirred solution of stannous chloride (82.5 grams) is concentrated HCl (230 ml.) at room temperature. Stirring is continued at room temperature for 1/2 hours, then the reaction mixture is cooled to 0° and made strongly basic with 50% NaOH. The reaction mixture is diluted with water (1 l.) and extracted four times with methylenechloride (200 ml.). The combined extracts are washed once with water (200 ml.), dried over sodium sulfate, then taken to dryness under reduced pressure. Recrystallization of the crude solid (4.6 grams) from benzene-Skellysolve B gives the product (4.15 grams) melting at 91°-92°.

後処理

  1. customat room temperature
  2. temperaturethe reaction mixture is cooled to 0°
  3. extractionextracted four times with methylenechloride (200 ml.)
  4. washThe combined extracts are washed once with water (200 ml.)
  5. dry with materialdried over sodium sulfate
  6. customRecrystallization of the crude solid (4.6 grams) from benzene-Skellysolve B

出典と根拠

ORDレコード
ord-1e71f419ff6e4266bc44b438fa361b29
出典データセット
uspto-grants-1976_05
特許番号
US03959289

反応ノート

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