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HCID 19850150, 화합물 → HCID 19850156, 화합물

HRID 1608011
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HRID 1608011 반응식
C(O[CH:4](OCC)[CH2:5][C:6]([NH:8][C:9]1[CH:14]=[C:13]([CH2:15][CH2:16][NH:17][C:18](=[O:23])[C:19]([F:22])([F:21])[F:20])[CH:12]=[CH:11][C:10]=1[O:24][CH3:25])=[O:7])C>S(=O)(=O)(O)O>[CH3:25][O:24][C:10]1[CH:11]=[CH:12][C:13]([CH2:15][CH2:16][NH:17][C:18](=[O:23])[C:19]([F:20])([F:21])[F:22])=[C:14]2[C:9]=1[NH:8][C:6](=[O:7])[CH:5]=[CH:4]2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 1

HCID 19850150HCID 19850150, 화합물

생성물 1

HCID 19850156HCID 19850156, 화합물수율 83.3%

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

실험 절차

The product of (a) (17.0 g, 42 mmoles) was added cautiously to concentrated sulphuric acid (50 ml) with stirring. When the addition was complete the dark solution was heated at 100° for 45 min then cooled and poured into ice-water. The suspension was extracted with ethyl acetate, and the extracts washed with sodium bicarbonate solution and water, dried and evaporated to give the sub-title compound as a pale yellow solid (11.0 g) mp 181°-184°. A sample recrystallised from ethanol-cyclohexane formed colourless needles mp 185°-186°.

후처리

  1. additionWhen the addition
  2. temperaturewas heated at 100° for 45 min
  • temperaturethen cooled
  • extractionThe suspension was extracted with ethyl acetate
  • washthe extracts washed with sodium bicarbonate solution and water
  • customdried
  • customevaporated
  • 출처 및 근거

    ORD 기록
    ord-f13419e04f824a07a2ed8e09e683dd70
    출처 데이터셋
    uspto-grants-1989_09
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US04868306

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