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Sulfuric Acid → HCID 19737996, 화합물

HRID 2255500
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HRID 2255500 반응식
S(=O)(=O)(O)[OH:2].CO[CH:8]1[C:13]2[CH:14]=[C:15]([S:17]([NH2:20])(=[O:19])=[O:18])[S:16][C:12]=2[S:11](=[O:22])(=[O:21])[N:10]([CH3:23])[CH2:9]1.[C:24](#[N:26])[CH3:25]>>[C:24]([NH:26][CH:8]1[C:13]2[CH:14]=[C:15]([S:17]([NH2:20])(=[O:18])=[O:19])[S:16][C:12]=2[S:11](=[O:21])(=[O:22])[N:10]([CH3:23])[CH2:9]1)(=[O:2])[CH3:25]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 1118Sulfuric AcidHCID 6342AcetonitrileHCID 18357855HCID 18357855, 화합물

생성물 1

HCID 19737996HCID 19737996, 화합물

실험 절차

To sulfuric acid (5.0 g) cooled to 0° C. was added the product from Step E (1.10 g, 3.81 mmol) dissolved in acetonitrile (35 mL) dropwise over 10 min. The mixture was stirred at ambient temperature for 2.5 days and quenched by the addition of ice and ammonium hydroxide to adjust the pH to 10. The acetonitrile was evaporated and the white precipitate was filtered and dried to give 0.41 g of the desired product. The filtrate was extracted with ethyl acetate. Evaporation to dryness gave an additional 0.33 g of the desired product (total yield 57%). Crystallization from methanol-methylene chloride gave colorless crystals: mp 252°-253° C.

후처리

custom
quenched by the addition of ice and ammonium hydroxide
  • customThe acetonitrile was evaporated
  • filtrationthe white precipitate was filtered
  • customdried
  • 출처 및 근거

    ORD 기록
    ord-54790b850f3549bbb7dbd2c4327e3a1c
    출처 데이터셋
    uspto-grants-1993_08
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US05240923

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