Hydrochloric Acid → HCID 53877200、化合物

HRID 126764

反応式

HRID 126764 の反応式
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]=[C:9]=[O:10])=[CH:4][CH:3]=1.[NH2:11][C:12](=[N:15][C:16](=O)[O:17]C)[S:13][CH3:14].C[O-].[Na+].Cl>C(Cl)Cl>[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[C:16](=[O:17])[NH:15][CH:12]([S:13][CH3:14])[NH:11][C:9]2=[O:10])=[CH:4][CH:3]=1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 693254-Methylphenyl isocyanateHCID 2935781-methoxycarbonyl-S-methylisothioureaHCID 10942334Sodium Methoxide

生成物 1

HCID 53877200HCID 53877200、化合物収率 81%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

4-Methylphenylisocyanate (19.0 g.) was added during 10 minutes to a solution of methyl N-[1-amino-1-(methylthio)methylene]carbamate (21.2 g.) in methylene chloride (200 ml.). After 2 hours of stirring, sodium methoxide [obtained by dissolving sodium (3.5 g.) in methanol (30 ml.)] was added at 15°-20° C. The subsequent mixture was stirred at that temperature for 18 hours and the resultant solid collected by filtration and dissolved in water (200 ml.). The solution obtained was acidified with concentrated hydrochloric acid and the solid which formed was collected by filtration, washed well with water and dried to give 3-(4-methylphenyl)-6-methylthiotetrahydro-1,3,5-triazine-2,4-dione (29 g., 81%), m.p. 276°-278° C.

後処理

  1. stirringThe subsequent mixture was stirred at that temperature for 18 hours
  2. filtrationthe resultant solid collected by filtration
  3. dissolutiondissolved in water (200 ml.)
  4. customThe solution obtained
  5. customthe solid which formed
  6. filtrationwas collected by filtration
  7. washwashed well with water
  8. customdried

出典と根拠

ORDレコード
ord-08bda83688d34e06852d475c07644bc7
出典データセット
uspto-grants-1981_03
特許番号
US04254122

関連ノート

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