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Tributylamine → HCID 13101160、化合物

HRID 543285
ノート
印刷プレビュー

反応式

HRID 543285 の反応式
Cl[C:2]1[S:3][C:4](Cl)=[C:5]2[C:11]=1[C:10](=[O:12])[C:9]1=[CH:13][S:14][CH:15]=[C:8]1[C:7](=[O:16])[NH:6]2.C(N(CCCC)CCCC)CCC.[H][H]>[Pd].C(O)CC>[CH:2]1[S:3][CH:4]=[C:5]2[C:11]=1[C:10](=[O:12])[C:9]1=[CH:13][S:14][CH:15]=[C:8]1[C:7](=[O:16])[NH:6]2
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 7622TributylamineHCID 13766010HCID 13766010、化合物HCID 178418361HCID 178418361、化合物

生成物 1

HCID 13101160HCID 13101160、化合物収率 75.2%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 10311-Propanol溶媒2 回

実験手順

A mixture of 5.0 g (0.0164 mole) of 1,3-dichloro-4,5-dihydrodithieno[3,4-b:3',4'-e]azepine-5,9-dione, 4 g of 5% strength Pd/C, 6.3 g (0.034 mole) of tributylamine and 300 ml of propanol was stirred in a hydrogen atmosphere at 80° C. When absorption of hydrogen was complete (after 5 hours), the hot mixture was filtered and the filtrate was poured onto ice water. The resulting suspension was acidified with concentrated hydrochloric acid, and the mixture was then stirred for a short time and filtered under suction. The residue from filtration of the crude reaction mixture was washed several times with hot dimethylformamide. The dimethylformamide used for washing was poured onto ice water, and the precipitate formed was filtered off under suction. The solid thus obtained was combined with the solid product obtained from the propanol filtrate. The total solid product was washed with water and then dried at 50° C. in a drying oven under reduced pressure. 2.9 g (75%) of 4,5-dihydrodithieno[3,4-b:3',4'-e]azepine-5,9-dione were obtained in the form of beige crystals of melting point 268°-271° C.

後処理

  1. customWhen absorption of hydrogen
  2. custom(after 5 hours)
  3. filtrationthe hot mixture was filtered
  4. additionthe filtrate was poured onto ice water
  5. filtrationfiltered under suction
  6. filtrationThe residue from filtration of the crude
  7. customreaction mixture
  8. washwas washed several times with hot dimethylformamide
  9. washfor washing
  10. additionwas poured onto ice water
  11. customthe precipitate formed
  12. filtrationwas filtered off under suction
  13. customThe solid thus obtained
  14. washThe total solid product was washed with water
  15. customdried at 50° C. in a drying oven under reduced pressure

出典と根拠

ORDレコード
ord-68ff66f7d98d41ec99d29bceba027f52
出典データセット
uspto-grants-1987_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04661591

反応ノート

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