Hydrochloric Acid → Biuret, 1-phenyl-2,4-dithio-

HRID 968881노트

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HRID 968881 반응식
[OH-].[Na+].[NH2:3][C:4]([NH2:6])=[S:5].[C:7]1([N:13]=[C:14]=[S:15])[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1.Cl>O.CC#N>[C:7]1([NH:13][C:14]([NH:3][C:4]([NH2:6])=[S:5])=[S:15])[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 7673Phenyl IsothiocyanateHCID 14798Sodium HydroxideHCID 2723790Thiourea

생성물 1

HCID 3032513Biuret, 1-phenyl-2,4-dithio-수율 30%

시약·촉매·용매 2

HCID 962Water용매HCID 6342Acetonitrile용매

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온도
40 °C

실험 절차

To a stirring solution of NaOH (0.52 g, 13.1 mmol) in 60 mL of 10% H2O:CH3CN was added thiourea (1.0 g, 13.1 mmol). The resulting suspension was heated to 40° C. for 20 min. and then cooled to RT. To this mixture was added phenylisothiocyanate (1.5 ml, 13.1 mmol), and the clear yellow solution was stirred overnight. After stirring for 12 h, 1 N HCl was added until a white precipitate formed. The precipitate was filtered, washed with H2O, and dried under vacuum to produce the title compound as a light yellow powder (0.78 g, 30%). 1H-NMR (400 MHz, d6-DMSO) δ7.25 (t, 2H, J=7.3 Hz), 7.40 (t, 2H, J=7.9 Hz), 7.56 (d, 1H, J=7.9 Hz), 9.13-9.29 (broad singlet, 1H), and 10.26-10.79 (broad singlet, 2H).

후처리

  1. temperaturecooled to RT
  2. stirringAfter stirring for 12 h
  3. customformed
  4. filtrationThe precipitate was filtered
  5. washwashed with H2O
  6. customdried under vacuum

출처 및 근거

ORD 기록
ord-348f13fa09404c4c813cd79233b41ba5
출처 데이터셋
uspto-grants-2007_12
특허 번호
US07304082B2

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