Hydrochloric Acid → (3-Aminophenyl)(3-methylphenyl)methanone

HRID 2231745ノート

反応式

HRID 2231745 の反応式
[CH3:1][C:2]1[CH:3]=[C:4]([CH:31]=[CH:32][CH:33]=1)[C:5]([C:7]1[CH:8]=[C:9]([NH:13]C(CC2C=CN3C=2CSC3C2C=NC=CC=2)=O)[CH:10]=[CH:11][CH:12]=1)=[O:6].CC1C=C(C(=O)C2C=CC=C([N+]([O-])=O)C=2)C=CC=1.Cl>C(O)C>[NH2:13][C:9]1[CH:8]=[C:7]([CH:12]=[CH:11][CH:10]=1)[C:5]([C:4]1[CH:31]=[CH:32][CH:33]=[C:2]([CH3:1])[CH:3]=1)=[O:6]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 21285581HCID 21285581、化合物HCID 131715768HCID 131715768、化合物

生成物 1

HCID 21285570(3-Aminophenyl)(3-methylphenyl)methanone

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
85 °C

実験手順

The 3-amino-3'-methylbenzophenone may be prepared as follows: stannous chloride in the dihydrate form(19 g) is added, at a temperature between 40° and 80° C., to a suspension of 3'-methyl-3-nitrobenzophenone (6.8 g) in a mixture of ethanol (80 cc) and concentrated hydrochloric acid (30 cc), in the course of 10 minutes. The solution obtained is heated at a temperature in the vicinity of 85° C. for 3 hours and then stirred at a temperature in the vicinity of 20° C. for 16 hours. The solvent is evaporated off under reduced pressure (20 mm Hg; 2.7 kPa) at a temperature in the vicinity of 60° C. The residue is suspended in distilled water (300 cc). An aqueous 10N sodium hydroxide solution (100 cc) is added, at a temperature in the vicinity of 20° C., with stirring, to the suspension obtained and extraction is carried out 3 times with diethyl ether (550 cc in total). The ether extracts are combined, washed twice with distilled water (300 cc in total) and then dried over anhydrous magnesium sulphate, treated with decolourizing charcoal (0.5 g), filtered and concentrated to dryness under reduced pressure (20 mm Hg; 2.7 kPa) at a temperature in the vicinity of 50° C. 3-Amino-3'-methylbenzophenone (5.7 g) in the form of yellow crystals, m.p. 110° C., is thereby obtained.

後処理

  1. customThe solution obtained
  2. customThe solvent is evaporated off under reduced pressure (20 mm Hg; 2.7 kPa) at a temperature in the vicinity of 60° C
  3. additionAn aqueous 10N sodium hydroxide solution (100 cc) is added, at a temperature in the vicinity of 20° C.
  4. stirringwith stirring, to the suspension
  5. customobtained
  6. extractionextraction
  7. washwashed twice with distilled water (300 cc in total)
  8. dry with materialdried over anhydrous magnesium sulphate
  9. additiontreated with decolourizing charcoal (0.5 g)
  10. filtrationfiltered
  11. concentrationconcentrated to dryness under reduced pressure (20 mm Hg; 2.7 kPa) at a temperature in the vicinity of 50° C

出典と根拠

ORDレコード
ord-b223f025862e4e92bd84628e86e5447c
出典データセット
uspto-grants-1988_11
特許番号
US04783472

反応ノート

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