Ethyl cyanoacetate → HCID 54413059, 화합물

HRID 1704729

반응식

HRID 1704729 반응식
CC[O-].[Na+].[C:5]([CH2:7][C:8](OCC)=[O:9])#[N:6].[C:13]1([CH:19]=[C:20]2[C:25](=[O:26])[C:24](=[CH:27][C:28]3[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=3)[CH2:23][S:22][CH2:21]2)[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1>CCO>[O:9]=[C:8]1[O:26][C:25]2[C:24](=[CH:27][C:28]3[CH:29]=[CH:30][CH:31]=[CH:32][CH:33]=3)[CH2:23][S:22][CH2:21][C:20]=2[CH:19]([C:13]2[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=2)[CH:7]1[C:5]#[N:6]

참가 물질

5

반응물 3

HCID 7764Ethyl cyanoacetateHCID 336779tetrahydro-3,5-bis(phenylmethylene)-4H-thiopyran-4-oneHCID 2723922Sodium ethoxide

생성물 1

HCID 54413059HCID 54413059, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

To a solution of NaOEt (from 555 mg, 92 mg atom Na in absolute EtOH) in 100 ml of absolute EtOH is added ethyl cyanoacetate (2.44 g, 22 mmole) dissolved in 50 ml of absolute EtOH. This is heated at reflux temperature for 2 hours, cooled slightly and tetrahydro-3,5-bis(phenylmethylene)-4H-thiopyran-4-one (5.84 g, 20 mmole) is added at once. The mixture quickly turns orange-red for ca. 10 minutes, changing to yellow (yellow solids in orange-red solution) as heating is continued for 2 hours.

후처리

  1. temperatureThis is heated
  2. temperatureat reflux temperature for 2 hours
  3. temperaturecooled slightly
  4. temperatureas heating
  5. waitis continued for 2 hours

출처 및 근거

ORD 기록
ord-b0cd7425e0bf47af9e85693cd6ceaf55
출처 데이터셋
uspto-grants-1978_11
특허 번호
US04127667

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