Formic Acid → N-[2-(7-methoxy-1,3-benzodioxol-5-yl)ethyl]formamide

HRID 1253109노트

반응식

HRID 1253109 반응식
Cl.[CH3:2][O:3][C:4]1[CH:5]=[C:6]([CH2:13][CH2:14][NH-:15])[CH:7]=[C:8]2[O:12][CH2:11][O:10][C:9]=12.[OH-].[Na+].[CH:18](O)=[O:19]>O>[CH3:2][O:3][C:4]1[CH:5]=[C:6]([CH2:13][CH2:14][NH:15][CH:18]=[O:19])[CH:7]=[C:8]2[O:12][CH2:11][O:10][C:9]=12

참가 물질

5

반응물 3

HCID 284Formic AcidHCID 14798Sodium HydroxideHCID 867421922-(3-Methoxy-4,5-methylenedioxyphenyl)ethylamide hydrochloride

생성물 1

HCID 10198394N-[2-(7-methoxy-1,3-benzodioxol-5-yl)ethyl]formamide수율 83%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

6.95 g (30 mmol) of 2-(3-methoxy-4,5-methylenedioxyphenyl)ethylamide hydrochloride was dissolved in 30 ml of water, and the mixture was made basic with 25% sodium hydroxide aqueous solution. The mixture was extracted with 30 ml of toluene. The toluene layer was washed with 10 ml of water, added with 2.73 g (59.3 mmol) of formic acid, refluxed under heating for 2 hours at normal pressure to distill off about 15 ml of the toluene while separating the produced water by an azeotropic distillation and then cooled. The deposited crystal was filtered out, washed with 3 ml of toluene and dried to obtain 5.48 g of N-[2-(3-methoxy-4,5-methylenedioxyphenyl)ethyl]formamide (C). Yield: 83%; melting point: 108°-110° C.

후처리

  1. extractionThe mixture was extracted with 30 ml of toluene
  2. washThe toluene layer was washed with 10 ml of water
  3. temperaturerefluxed
  4. temperatureunder heating for 2 hours at normal pressure
  5. distillationto distill off about 15 ml of the toluene
  6. customwhile separating the produced water
  7. distillationby an azeotropic distillation
  8. temperaturecooled
  9. filtrationThe deposited crystal was filtered out
  10. washwashed with 3 ml of toluene
  11. customdried

출처 및 근거

ORD 기록
ord-0c793d2906a54f72b6fcb4757a104709
출처 데이터셋
uspto-grants-1988_05
특허 번호
US04746747

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