Hydrochloric Acid → 4,6-Dichlorobenzene-1,3-diamine

HRID 236937

反応式

HRID 236937 の反応式
Cl.[Cl:2][C:3]1[CH:8]=[C:7]([Cl:9])[C:6]([N+:10]([O-])=O)=[CH:5][C:4]=1[N+:13]([O-])=O.[OH-].[Na+]>>[NH2:13][C:4]1[C:3]([Cl:2])=[CH:8][C:7]([Cl:9])=[C:6]([NH2:10])[CH:5]=1

参加物

4

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 772861,3-Dichloro-4,6-dinitrobenzene

生成物 1

HCID 33728694,6-Dichlorobenzene-1,3-diamine

実験手順

To a solution of 399 gm. (1.77 mole) of stannous chloride dihydrate in 975 ml. of concentrated hydrochloric acid is added 60 gm. (0.258 mole) of 1,5-dichloro-2,4-dinitrobenzene. The temperature rises to 72° and a solution occurs. The mixture is allowed to cool to room temperature and then cooled in an ice-bath (to 5°). A cold 50% solution of sodium hydroxide is added, with cooling, until the mixture is strongly basic. The mixture is filtered and the precipitate on the funnel washed four times with 500 ml. portions of ethyl acetate. The ethyl acetate extracts are combined, dried over anhydrous M9SO4 and the solvent removed. The residue is recrystallized from 50% ethanol-water. There is obtained 31.9 gm. (70%) of colorless needles melting at 142-3°.

後処理

  1. customrises to 72°
  2. temperaturecooled in an ice-bath (to 5°)
  3. temperaturewith cooling, until the mixture
  4. filtrationThe mixture is filtered
  5. washthe precipitate on the funnel washed four times with 500 ml
  6. customdried over anhydrous M9SO4
  7. customthe solvent removed
  8. customThe residue is recrystallized from 50% ethanol-water
  9. customThere is obtained 31.9 gm

出典と根拠

ORDレコード
ord-cf0fbddac1074383a6b5e63e410f16e2
出典データセット
uspto-grants-1979_06
特許番号
US04159278

関連ノート

読み込み中…