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

HRID 968881ノート

反応式

HRID 968881 の反応式
[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

参加物

7

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6342Acetonitrile溶媒

反応条件

温度
40 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-348f13fa09404c4c813cd79233b41ba5
出典データセット
uspto-grants-2007_12
特許番号
US07304082B2

反応ノート

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