Acetic Acid → HCID 66921947, 화합물

HRID 1361470노트

반응식

HRID 1361470 반응식
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]

참가 물질

7

반응물 4

HCID 176Acetic Acid2회HCID 807IodineHCID 1004Phosphoric AcidHCID 30165104-Amino-2,4'-dichlorobenzophenone

생성물 1

HCID 66921947HCID 66921947, 화합물수율 100%

시약·촉매·용매 2

HCID 962Water용매HCID 8857Ethyl Acetate용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-7ce953cc1aa84ee8b28dbd47419eca39
출처 데이터셋
uspto-grants-2011_02
특허 번호
US07880006B2

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