Hydrochloric Acid → 4-Amino-2,4'-dichlorobenzophenone

HRID 1361469ノート

反応式

HRID 1361469 の反応式
O.Cl.[Cl:3][C:4]1[CH:9]=[C:8]([N+:10]([O-])=O)[CH:7]=[CH:6][C:5]=1[C:13]([C:15]1[CH:20]=[CH:19][C:18]([Cl:21])=[CH:17][CH:16]=1)=[O:14].O.C(=O)(O)[O-].[Na+]>C(O)C.[Fe]>[NH2:10][C:8]1[CH:7]=[CH:6][C:5]([C:13]([C:15]2[CH:20]=[CH:19][C:18]([Cl:21])=[CH:17][CH:16]=2)=[O:14])=[C:4]([Cl:3])[CH:9]=1

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 8862964-Chlorophenyl 2-chloro-4-nitrophenyl ketoneHCID 86585896Sodium bicarbonate water

生成物 1

HCID 30165104-Amino-2,4'-dichlorobenzophenone収率 95%

試薬・触媒・溶媒 2

HCID 23925Iron触媒HCID 702Ethanol溶媒2 回

実験手順

Iron powder (12 g), 42 mL of ethanol, 17 mL of distilled water, and 0.09 mL of 35% hydrochloric acid were mixed together, and the mixture was heated to reflux. Subsequently, (2-chloro-4-nitrophenyl)-(4′-chlorophenyl)methanone (8.9 g) dissolved in 12.8 mL of ethanol was added dropwise to the mixed solution, and the mixture was heated under reflux for one hr. This mixed solution was then cooled to room temperature, sodium bicarbonate water was then added thereto, and the mixture was filtered. The filtrate was concentrated under the reduced pressure, and ethyl acetate and brine were added to the residue, followed by separation. The ethyl acetate layer was washed with brine and was then concentrated under the reduced pressure to give 7.56 g of (4-amino-2-chlorophenyl)-(4′-chlorophenyl)methanone (yield 95%).

後処理

  1. temperaturethe mixture was heated to reflux
  2. additionwas added dropwise to the mixed solution
  3. temperaturethe mixture was heated
  4. temperatureunder reflux for one hr
  5. filtrationthe mixture was filtered
  6. concentrationThe filtrate was concentrated under the reduced pressure, and ethyl acetate and brine
  7. additionwere added to the residue
  8. customfollowed by separation
  9. washThe ethyl acetate layer was washed with brine
  10. concentrationwas then concentrated under the reduced pressure

出典と根拠

ORDレコード
ord-05d617c07cff4d08b82b9222c8ff663f
出典データセット
uspto-grants-2011_02
特許番号
US07880006B2

反応ノート

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