Water → 3,4-dihydrothieno[3,2-f][1,4]thiazepin-5(2H)-one

HRID 847384ノート

反応式

HRID 847384 の反応式
[S:1]1[C:5]2[S:6][CH2:7][CH2:8][C:9](=[N:10]O)[C:4]=2[CH:3]=[CH:2]1.[OH2:12]>>[S:6]1[C:5]2[S:1][CH:2]=[CH:3][C:4]=2[C:9](=[O:12])[NH:10][CH2:8][CH2:7]1

参加物

3

反応物 2

HCID 962WaterHCID 27397394H-Thieno[2,3-b]thiopyran-4-one, 5,6-dihydro-, oxime

生成物 1

HCID 43659423,4-dihydrothieno[3,2-f][1,4]thiazepin-5(2H)-one

実験手順

To 300 g of polyphosphoric acid warmed at 70° C. was added 19.5 g of 5,6-dihydro-4H-thieno[2,3-b]thiopyran-4-one 4-oxime portionwise with stirring for 20 minutes. The mixture was stirred at 80° C. for 2.5 hours, poured into chilled water and extracted with chloroform. The extract was washed with water, dried over magnesium sulfate and concentrated under reduced pressure. The resulting crude crystals were recrystallized from ethanol to give 10 g of 2,3-dihydrothieno[3,2-f]-1,4-thiazepin-5(4H)-one as white crystals, melting at 195°-196° C.

後処理

  1. stirringThe mixture was stirred at 80° C. for 2.5 hours
  2. additionpoured
  3. extractionextracted with chloroform
  4. washThe extract was washed with water
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated under reduced pressure
  7. customThe resulting crude crystals were recrystallized from ethanol

出典と根拠

ORDレコード
ord-33947bbe19144a7bbe461df9a64614ab
出典データセット
uspto-grants-1992_08
特許番号
US05141930

反応ノート

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