1-[4-Chloro-2-benzoylphenyl]-3-phthalimidopropyne → HCID 13556875、化合物

HRID 464929ノート

反応式

HRID 464929 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]#[C:9][CH2:10][N:11]2[C:15](=[O:16])[C:14]3=[CH:17][CH:18]=[CH:19][CH:20]=[C:13]3[C:12]2=[O:21])=[C:4]([C:22](=[O:29])[C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)[CH:3]=1>[Ni].O1CCCC1>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][CH2:9][CH2:10][N:11]2[C:15](=[O:16])[C:14]3=[CH:17][CH:18]=[CH:19][CH:20]=[C:13]3[C:12]2=[O:21])=[C:4]([C:22](=[O:29])[C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)[CH:3]=1

参加物

4

反応物 1

HCID 128782521-[4-Chloro-2-benzoylphenyl]-3-phthalimidopropyne

生成物 1

HCID 13556875HCID 13556875、化合物

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 8028Tetrahydrofuran溶媒

実験手順

A mixture of 2 g (5 mmole) of 1-[4-chloro-2-benzoylphenyl]-3-phthalimidopropyne and 1/2 teaspoonful of Raney nickel in 25 ml of tetrahydrofuran was hydrogenated at room temperature and atmospheric pressure. When 240 ml of hydrogen was absorbed, the catalyst was separated by filtration and the filtrate concentrated at reduced pressure to dryness. The residue was crystallized from a mixture of ether and petroleum to give crude product as a tan solid, mp 94°-97° C. Recrystallization from ether gave pale yellow prisms, mp 98°-99° C.

後処理

  1. customwas hydrogenated at room temperature
  2. customWhen 240 ml of hydrogen was absorbed
  3. customthe catalyst was separated by filtration
  4. concentrationthe filtrate concentrated at reduced pressure to dryness
  5. customThe residue was crystallized from a mixture of ether and petroleum
  6. customto give crude product as a tan solid, mp 94°-97° C
  7. customRecrystallization from ether
  8. customgave pale yellow prisms, mp 98°-99° C.

出典と根拠

ORDレコード
ord-5dac1004c7aa4f46a545bfd9442e133f
出典データセット
uspto-grants-1985_10
特許番号
US04549988

反応ノート

読み込み中…