Pyridine → HCID 13390867、化合物

HRID 1731604ノート

反応式

HRID 1731604 の反応式
[S:1]1(=[O:11])(=[O:10])[C:5]2=[CH:6][S:7][CH:8]=[C:4]2[C:3](=O)[NH:2]1.N1C=CC=CC=1.P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:19]>O>[S:1]1(=[O:11])(=[O:10])[C:5]2=[CH:6][S:7][CH:8]=[C:4]2[C:3](=[S:19])[NH:2]1

参加物

5

反応物 3

HCID 1049PyridineHCID 14817Phosphorus sulfide (P2S5)HCID 12593672thieno[3,4-d]isothiazol-3(2H)-one 1,1-dioxide

生成物 1

HCID 13390867HCID 13390867、化合物収率 40%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
80 °C

実験手順

To a mixture of 5.6 g. (0.03 mole) of thieno[3,4-d]isothiazol-3(2H)-one 1,1-dioxide* in 50 ml. of dry pyridine is added 5.6 g. (0.016 mole) of phosphorus pentasulfide portionwise over 3 minutes. The viscous mixture is slowly heated in an oil bath under an atmosphere of nitrogen. The temperature of the oil bath is slowly increased to 80° C. after 30 minutes. The temperature of the oil bath is then kept at 80° C. for 25 minutes, the internal temperature reading 63° C. The solution is cooled to 50° C. and is added dropwise over 5 minutes to 200 ml. of water and cooled in an ice bath. The precipitate which forms is collected and discarded. The filtrate is cooled in ice and acidified with concentrated hydrochloric acid to pH 1. The precipitate which forms is collected to yield 40% of material. In another expeirment, a sample is recrystallized from water to obtain an analytical sample, m.p. 196°-8° C. (dec.).

後処理

  1. additionTo a mixture of 5.6 g
  2. temperatureThe viscous mixture is slowly heated in an oil bath under an atmosphere of nitrogen
  3. customreading 63° C
  4. temperatureThe solution is cooled to 50° C.
  5. additionis added dropwise over 5 minutes to 200 ml
  6. customThe precipitate which forms is collected
  7. temperatureThe filtrate is cooled in ice
  8. customThe precipitate which forms is collected

出典と根拠

ORDレコード
ord-1413e65883e64e67ac771871008a417f
出典データセット
uspto-grants-1986_11
特許番号
US04622402

反応ノート

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