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

HRID 1253109ノート

反応式

HRID 1253109 の反応式
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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-0c793d2906a54f72b6fcb4757a104709
出典データセット
uspto-grants-1988_05
特許番号
US04746747

反応ノート

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