Acetic Acid → HCID 66921947、化合物

HRID 1361470ノート

反応式

HRID 1361470 の反応式
II.C(O)(=O)C.P(=O)(O)(O)O.[NH2:12][C:13]1[CH:18]=[CH:17][C:16]([C:19]([C:21]2[CH:26]=[CH:25][C:24]([Cl:27])=[CH:23][CH:22]=2)=O)=[C:15]([Cl:28])[CH:14]=1>C(OCC)(=O)C.O>[Cl:28][C:15]1[CH:14]=[C:13]([CH:18]=[CH:17][C:16]=1[CH2:19][C:21]1[CH:26]=[CH:25][C:24]([Cl:27])=[CH:23][CH:22]=1)[NH2:12]

参加物

7

反応物 4

HCID 176Acetic Acid2 回HCID 807IodineHCID 1004Phosphoric AcidHCID 30165104-Amino-2,4'-dichlorobenzophenone

生成物 1

HCID 66921947HCID 66921947、化合物収率 100%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8857Ethyl Acetate溶媒

実験手順

Iodine (1 g) and 50 mL of acetic acid were mixed together, 2.53 g of 50% phosphoric acid was added thereto, and the mixture was heated with stirring to reflux. Subsequently, a mixture composed of 3.2 g of (4-amino-2-chlorophenyl)-(4′-chlorophenyl)methanone and 15 mL of acetic acid were added dropwise to the mixed solution. This solution was heated under reflux for 134 hr, was then cooled and was poured into water. Ethyl acetate was added to the mixed solution followed by separation and washing with brine. The ethyl acetate layer was concentrated to give 3.0 g of 3-chloro-4-(4-chlorobenzyl)aniline (yield 100%).

後処理

  1. temperaturethe mixture was heated
  2. temperatureto reflux
  3. additionwere added dropwise to the mixed solution
  4. temperatureThis solution was heated
  5. temperatureunder reflux for 134 hr
  6. temperaturewas then cooled
  7. customfollowed by separation
  8. washwashing with brine
  9. concentrationThe ethyl acetate layer was concentrated

出典と根拠

ORDレコード
ord-7ce953cc1aa84ee8b28dbd47419eca39
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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