3-Propylaniline → HCID 19829931, 화합물

HRID 1493609

반응식

HRID 1493609 반응식
[CH2:1]([C:4]1[CH:5]=[C:6]([CH:8]=[CH:9][CH:10]=1)[NH2:7])[CH2:2][CH3:3].C(=O)(O)[O-].[Na+].Cl[CH2:17][C:18]([O:20][CH3:21])=[O:19]>CCOCC>[CH3:21][O:20][C:18](=[O:19])[CH2:17][NH:7][C:6]1[CH:8]=[CH:9][CH:10]=[C:4]([CH2:1][CH2:2][CH3:3])[CH:5]=1

참가 물질

5

반응물 3

HCID 60563-PropylanilineHCID 7295Methyl chloroacetateHCID 516892Sodium Bicarbonate

생성물 1

HCID 19829931HCID 19829931, 화합물

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

3-n-Propyl-aniline (20 g, 148 mmol), sodium bicarbonate (24.9 g, 296 mmol) and methyl chloroacetate (24.0 g, 221 mmol) were mixed under nitrogen and stirred at 80°-90° C. for 24 h. The cooled reaction was poured into ether (100 ml) and filtered. The filtrate was washed with water (100 ml), dilute hydrochloric acid (100 ml) and water (100 ml), then dried and concentrated in vacuo. The oily product (21.2 g) was distilled on the Kugelrohr collecting the fraction boiling at 160°/0.35 mmHg to give the title compound (Intermediate 32) as a colourless liquid which solidified into a pale yellow, low melting solid (16.1 g, 53%).

후처리

  1. customThe cooled reaction
  2. filtrationfiltered
  3. washThe filtrate was washed with water (100 ml), dilute hydrochloric acid (100 ml) and water (100 ml)
  4. customdried
  5. concentrationconcentrated in vacuo
  6. distillationThe oily product (21.2 g) was distilled on the Kugelrohr
  7. customcollecting the fraction boiling at 160°/0.35 mmHg

출처 및 근거

ORD 기록
ord-834a1ce188ab48e48d7cd9f817d0fb93
출처 데이터셋
uspto-grants-1991_06
특허 번호
US05023255

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