1,4-Dioxane → HCID 20038701, 화합물

HRID 1393639노트

반응식

HRID 1393639 반응식
[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]

참가 물질

5

반응물 3

HCID 312751,4-DioxaneHCID 12896473Azane;hydrateHCID 23091968HCID 23091968, 화합물

생성물 1

HCID 20038701HCID 20038701, 화합물수율 81%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-f8213438ade54b82b880066a0d1e47dd
출처 데이터셋
uspto-grants-2008_03
특허 번호
US07345180B2

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