Ammonia → HCID 10986637, 화합물

HRID 1707359노트

반응식

HRID 1707359 반응식
C[O:2][C:3](=O)/[C:4](/Cl)=[C:5](\[O:7][CH3:8])/[CH3:6].[OH-].[Na+].[CH:13](=O)[CH:14]([CH3:16])[CH3:15].[NH3:18]>>[CH:13](=[C:6]1/[C:5]([O:7][CH3:8])=[CH:4][C:3](=[O:2])[NH:18]/1)\[CH:14]([CH3:16])[CH3:15]

참가 물질

5

반응물 4

HCID 222Ammonia2회HCID 6561IsobutyraldehydeHCID 14798Sodium Hydroxide2회HCID 5463552HCID 5463552, 화합물

생성물 1

HCID 10986637HCID 10986637, 화합물

실험 절차

120 g of (E)-2-chloro-3-methoxybut-2-enoic acid methyl ester was instilled in 200 ml of concentrated aqueous ammonia solution at 65° to 70° C. with constant passing through of ammonia gas within 3 hours. The reaction mixture was stirred another 1.5 hours at this temperature and then refluxed another 0.5 hour. After cooling to room temperature, 450 ml of 1M sodium hydroxide solution was added and the pH was brought to greater than 13 by the further addition of 33 percent sodium hydroxide solution. Then 50 g of isobutyraldehyde was added and the reaction mixture was heated to 60° C. with stirring for 6 hours. After cooling to room temperature, the precipitated product was filtered off, washed with cold water and dried in a vacuum drying cabinet. The yield of the title compound was 93.2 g (80 percent of theory). The title compound had a melting point of 140.5° to 141.1° C. (from diethyl ether).

후처리

  1. temperaturerefluxed another 0.5 hour
  2. temperaturethe reaction mixture was heated to 60° C.
  3. stirringwith stirring for 6 hours
  4. temperatureAfter cooling to room temperature
  5. filtrationthe precipitated product was filtered off
  6. washwashed with cold water
  7. customdried in a vacuum
  8. customdrying cabinet

출처 및 근거

ORD 기록
ord-d9d930c8d3d045a491bcf44bf562c59a
출처 데이터셋
uspto-grants-1994_10
특허 번호
US05352801

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