HCID 20406152, 화합물 → Methanone, (2-amino-5-methylphenyl)(4-fluorophenyl)-

HRID 2164305노트

반응식

HRID 2164305 반응식
[F:1][C:2]1[CH:20]=[CH:19][C:5]([C:6]([C:8]2[CH:13]=[C:12]([CH3:14])[CH:11]=[CH:10][C:9]=2[NH:15]C(=O)C)=[O:7])=[CH:4][CH:3]=1>C(O)C.Cl>[NH2:15][C:9]1[CH:10]=[CH:11][C:12]([CH3:14])=[CH:13][C:8]=1[C:6]([C:5]1[CH:19]=[CH:20][C:2]([F:1])=[CH:3][CH:4]=1)=[O:7]

참가 물질

4

반응물 1

HCID 20406152HCID 20406152, 화합물

생성물 1

HCID 10966280Methanone, (2-amino-5-methylphenyl)(4-fluorophenyl)-수율 61.5%

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매HCID 702Ethanol용매

실험 절차

A solution of 119 g (0.44 mole of N-[2-(4-fluorobenzoyl)-4-methylphenyl]acetamide in 500 ml of 95% ethanol and 300 ml of 6N hydrochloric acid was heated at reflux for 16 hr. The solvents were removed on a roto-evaporator and the residue obtained was partitioned between concentrated ammonium hydroxide and benzene. The organic layer was concentrated and the new residue was chromatographed on silica gel, eluting with 10% ethyl acetate in hexane. The product fractions were concentrated and the residue was crystallized from a mixture of cyclohexane and hexane to give 56.3 g (61.5%) of the titled compound as bright yellow crystals, m.p. 70.0°-71.5° C.

후처리

  1. temperatureat reflux for 16 hr
  2. customThe solvents were removed on a roto-evaporator
  3. customthe residue obtained
  4. customwas partitioned between concentrated ammonium hydroxide and benzene
  5. concentrationThe organic layer was concentrated
  6. customthe new residue was chromatographed on silica gel
  7. washeluting with 10% ethyl acetate in hexane
  8. concentrationThe product fractions were concentrated
  9. customthe residue was crystallized from a mixture of cyclohexane and hexane

출처 및 근거

ORD 기록
ord-ce1a0d64d9574e01bf7a2c3c022d8ff6
출처 데이터셋
uspto-grants-1985_03
특허 번호
US04503073

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