Formaldehyde → 5-dimethylaminomethyl-5,6-dihydro-4H-thieno[2,3-b]thiopyran-4-one hydrochloride

HRID 1586712ノート

反応式

HRID 1586712 の反応式
[S:1]1[C:5]2[S:6][CH2:7][CH2:8][C:9](=[O:10])[C:4]=2[CH:3]=[CH:2]1.[CH2:11]=O.[ClH:13].[CH3:14][NH:15][CH3:16]>C(O)(=O)C>[ClH:13].[CH3:14][N:15]([CH2:11][CH:8]1[CH2:7][S:6][C:5]2[S:1][CH:2]=[CH:3][C:4]=2[C:9]1=[O:10])[CH3:16]

参加物

5

反応物 3

HCID 712FormaldehydeHCID 10473Dimethylamine, hydrochlorideHCID 110302745,6-Dihydro-4H-thieno[2,3-b]thiopyran-4-one

生成物 1

HCID 126753075-dimethylaminomethyl-5,6-dihydro-4H-thieno[2,3-b]thiopyran-4-one hydrochloride収率 83.5%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
100 °C

実験手順

A mixture of 5,6-dihydrothieno[2,3-b]thiopyran-4-one (12.5 g, 0.074 mol), paraformaldehyde (7.5 g, 0.25 mol), dimethylamine-hydrochloride (40 g, 0.49 mol) and acetic acid (2 ml) was heated with stirring at 100° C. for 1 hour. After allowing to cool to room temperature, the solid was triturated with ethanol and the solid was collected on a filter to yield 16.3 g (83%) of the title compound. An analytical sample was prepared by crystallization from 95% ethanol and filtration through a pad of norite-ducco-supercel to yield product with mp 155°-157° C. Anal. Calc'd. for C10H13NOS2.HCl.

後処理

  1. temperaturewas heated
  2. temperatureto cool to room temperature
  3. customthe solid was triturated with ethanol
  4. customthe solid was collected on
  5. filtrationa filter

出典と根拠

ORDレコード
ord-1b9973f655274e1f9adf7e037a0fe2a9
出典データセット
uspto-grants-1993_06
特許番号
US05215989

反応ノート

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