1,3-Diethyl 2-oxopropanedioate → HCID 14152291, 화합물

HRID 579834노트

반응식

HRID 579834 반응식
[Cl:1][C:2]1[CH:11]=[CH:10][C:5]2[NH:6][CH2:7][CH2:8][O:9][C:4]=2[CH:3]=1.[O:12]=[C:13]([C:19](OCC)=[O:20])[C:14]([O:16][CH2:17][CH3:18])=[O:15].C(=O)([O-])[O-].[NH4+].[NH4+]>C(O)(=O)C>[Cl:1][C:2]1[CH:3]=[C:4]2[O:9][CH2:8][CH2:7][N:6]3[C:19](=[O:20])[C:13]([OH:12])([C:14]([O:16][CH2:17][CH3:18])=[O:15])[C:10]([CH:11]=1)=[C:5]23

참가 물질

5

반응물 3

HCID 691051,3-Diethyl 2-oxopropanedioateHCID 517111Ammonium CarbonateHCID 136432417-Chloro-3,4-dihydro-2H-1,4-benzoxazine

생성물 1

HCID 14152291HCID 14152291, 화합물수율 77.3%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

7-Chloro-3,4-dihydro-2H-1,4-benzoxazine (Japan Kokai JP No. 61-152984, U.S. Pat. No. 4,593,092) (19.77 g. 0.116 mol) was dissolved in 74 ml of acetic acid and to which diethyl ketomalonate 20.2 g (0.116 mol) was added dropwise at a room temperature. Then after refluxing for 20 minutes, the mixture was stand for overnight. After pouring into 500 ml of ice, ammonium carbonate was added to the solution. The resultant crystalline solid was collected by filtration, washed with water and dried to yield pale orange powders quantitatively. Recrystallization from ethanol afforded 26.67 g (77.3%) of the title compound as pale yellow prisms, mp 186°-187° C.

후처리

  1. additionwas added dropwise at a room temperature
  2. temperatureThen after refluxing for 20 minutes
  3. customfor overnight
  4. additionwas added to the solution
  5. filtrationThe resultant crystalline solid was collected by filtration
  6. washwashed with water
  7. customdried
  8. customto yield pale orange powders quantitatively
  9. customRecrystallization from ethanol

출처 및 근거

ORD 기록
ord-91bfceae01904600b7777ac9cd0465cf
출처 데이터셋
uspto-grants-1988_06
특허 번호
US04749789

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