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HCID 19101019, 화합물 → HCID 53683293, 화합물

HRID 1975223
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HRID 1975223 반응식
[NH2:1][C:2]1[O:7][C:6]2[C:8]3[C:13]([CH:14]=[CH:15][C:5]=2[CH:4]([C:16]2[CH:21]=[CH:20][C:19]([F:22])=[C:18]([Cl:23])[CH:17]=2)[C:3]=1[C:24]#[N:25])=[CH:12][CH:11]=[CH:10][CH:9]=3>C(OCC)(OCC)OCC>[Cl:23][C:18]1[CH:17]=[C:16]([CH:4]2[C:3]([C:24]#[N:25])=[C:2]([N:1]=[CH:2][O:7][CH2:6][CH3:5])[O:7][C:6]3[C:8]4[C:13]([CH:14]=[CH:15][C:5]2=3)=[CH:12][CH:11]=[CH:10][CH:9]=4)[CH:21]=[CH:20][C:19]=1[F:22]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 1

HCID 19101019HCID 19101019, 화합물

생성물 1

HCID 53683293HCID 53683293, 화합물

시약·촉매·용매 1

HCID 31214Ethyl orthoformate용매

실험 절차

2-Amino-4-(3-chloro-4-fluorophenyl)-4H-naphtho[1,2-b]pyran-3-carbonitrile (3.12 g) was heated, under reflux, in triethyl orthoformate (40 ml) for 24 hours. A fraction coming over at 80° to 140° C. was distilled off and more triethyl orthofomate (40 ml) was added, and the refluxing was continued for a further 24 hours. The solution was evaporated to dryness. The gummy residue was dissolved in chloroform and passed through a column of `flash` silica using 30% hexane in chloroform as eluant. The fractions containing product were bulked, evaporated and triturated with ethyl acetate to give white crystals of 4-(3-chloro-4-fluorophenyl)-2-ethoxymethyleneamino-4H-naphtho[1,2-b]pyran-3-carbonitrile, m.p. 146°-148° C.

후처리

  1. custom
coming over at 80° to 140° C.
  • distillationwas distilled off
  • additionmore triethyl orthofomate (40 ml) was added
  • customThe solution was evaporated to dryness
  • dissolutionThe gummy residue was dissolved in chloroform
  • additionThe fractions containing product
  • customevaporated
  • customtriturated with ethyl acetate
  • 출처 및 근거

    ORD 기록
    ord-6dedee11992c4fbca5dca97fd6e138ed
    출처 데이터셋
    uspto-grants-1994_02
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US05284868

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