1,4-Dioxane → HCID 20038701、化合物

HRID 1393639ノート

反応式

HRID 1393639 の反応式
[S:1]1[CH2:5][CH:4]([C:6]([O-])=[O:7])[N:3]([C:9]([O:11][C:12]([CH3:15])([CH3:14])[CH3:13])=[O:10])[CH2:2]1.O1CCOCC1.O.[NH3:23]>O1CCCC1>[C:6]([CH:4]1[CH2:5][S:1][CH2:2][N:3]1[C:9]([O:11][C:12]([CH3:15])([CH3:14])[CH3:13])=[O:10])(=[O:7])[NH2:23]

参加物

5

反応物 3

HCID 312751,4-DioxaneHCID 12896473Azane;hydrateHCID 23091968HCID 23091968、化合物

生成物 1

HCID 20038701HCID 20038701、化合物収率 81%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

3-t-Butyl thiazolidine-3,4-dicarboxylate (2.0 g) was dissolved in tetrahydrofuran (10 ml), and N,N′-carbonyl diimidazole (1.4 g) was added thereto with ice-cooling. The mixture was warmed to room temperature and stirred for 6 hours. 1,4-Dioxane (10 ml) was added thereto, and the mixture was added dropwise to 28% ammonia water (40 ml) cooled on an ice bath. The mixture was warmed to room temperature and stirred for 20 hours. The reaction solution was extracted with ethyl acetate (60 ml). The organic phase was washed with a saturated saline solution and dried over sodium sulfate anhydrous. The product was concentrated under reduced pressure to give t-butyl 4-carbamoylthiazolidine-3-carboxylate (1.6 g, Y.:81%).

後処理

  1. temperaturewith ice-cooling
  2. temperaturecooled on an ice bath
  3. temperatureThe mixture was warmed to room temperature
  4. stirringstirred for 20 hours
  5. extractionThe reaction solution was extracted with ethyl acetate (60 ml)
  6. washThe organic phase was washed with a saturated saline solution
  7. dry with materialdried over sodium sulfate anhydrous
  8. concentrationThe product was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-f8213438ade54b82b880066a0d1e47dd
出典データセット
uspto-grants-2008_03
特許番号
US07345180B2

反応ノート

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