HCID 13067091, 화합물 → HCID 13067111, 화합물

HRID 223483노트

반응식

HRID 223483 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:9]([C:14]#[N:15])=[CH:10][NH:11][C:12]=2[CH3:13])=[C:4]([C:16](=O)[C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=2[Cl:23])[CH:3]=1>[Ni].C(O)(=O)C>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]2[C:8]3[C:9](=[CH:10][NH:11][C:12]=3[CH3:13])[CH2:14][N:15]=[C:16]([C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=3[Cl:23])[C:4]=2[CH:3]=1

참가 물질

4

반응물 1

HCID 13067091HCID 13067091, 화합물

생성물 1

HCID 13067111HCID 13067111, 화합물

시약·촉매·용매 2

HCID 935Nickel촉매HCID 176Acetic Acid용매

실험 절차

A mixture of 8.5 g (24 mmol) of 4-[4-chloro-2-(2-chlorobenzoyl)phenyl]-5-methyl-1H-pyrrole-3-carbonitrile, 1 spoonful of Raney nickel and 250 ml of glacial acetic acid was hydrogenated on a Parr apparatus at 55 psi overnight. The catalyst was removed by filtration and the acetic acid was removed at reduced pressure. The residue was diluted with water, basified with concentrated ammonium hydroxide and the resulting precipitate was collected by filtration. The precipitate was dissolved in tetrahydrofuran, dried over anhydrous sodium sulfate and concentrated at reduced pressure. The residue was crystallized from a mixture of ether and petroleum ether to give off-white crystals (mp 219°-222°). Recrystallization from a mixture of ether and methylene chloride gave colorless crystals, mp 221°-225°.

후처리

  1. customwas hydrogenated on a Parr apparatus at 55 psi overnight
  2. customThe catalyst was removed by filtration
  3. customthe acetic acid was removed at reduced pressure
  4. additionThe residue was diluted with water
  5. filtrationthe resulting precipitate was collected by filtration
  6. dissolutionThe precipitate was dissolved in tetrahydrofuran
  7. dry with materialdried over anhydrous sodium sulfate
  8. concentrationconcentrated at reduced pressure
  9. customThe residue was crystallized from a mixture of ether and petroleum ether

출처 및 근거

ORD 기록
ord-fcd6ddefbd3148a69121ae4072cd6e9a
출처 데이터셋
uspto-grants-1982_10
특허 번호
US04354973

반응 노트

불러오는 중…