1-[4-Chloro-2-benzoylphenyl]-3-phthalimidopropyne → HCID 13556875, 화합물

HRID 464929노트

반응식

HRID 464929 반응식
[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

참가 물질

4

반응물 1

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

생성물 1

HCID 13556875HCID 13556875, 화합물

시약·촉매·용매 2

HCID 935Nickel촉매HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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.

출처 및 근거

ORD 기록
ord-5dac1004c7aa4f46a545bfd9442e133f
출처 데이터셋
uspto-grants-1985_10
특허 번호
US04549988

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