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2-Methoxyaniline → N-(4-methyl-1,3-dioxolan-2-ylmethyl)-2-methoxyaniline

HRID 28045
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HRID 28045 반응식
[CH3:1][O:2][C:3]1[CH:9]=[CH:8][CH:7]=[CH:6][C:4]=1[NH2:5].C(=O)([O-])[O-].[Na+].[Na+].Br[CH2:17][CH:18]1[O:22][CH:21]([CH3:23])[CH2:20][O:19]1>>[CH3:23][CH:21]1[CH2:20][O:19][CH:18]([CH2:17][NH:5][C:4]2[CH:6]=[CH:7][CH:8]=[CH:9][C:3]=2[O:2][CH3:1])[O:22]1
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참가 물질

4

반응물 3

HCID 70002-MethoxyanilineHCID 10340Sodium CarbonateHCID 141307cis-2-Bromomethyl-4-methyl-1,3-dioxolane

생성물 1

HCID 23338376N-(4-methyl-1,3-dioxolan-2-ylmethyl)-2-methoxyaniline

반응 조건

온도
100 °C

실험 절차

2-Methoxyaniline (99 grams; 0.6 moles) and sodium carbonate (31.6 grams) were charged into a glass reaction vessel equipped with a mechanical stirrer, thermometer and reflux condenser. 2-Bromomethyl-4-methyl-1,3-dioxolane (25 ml) was added and the reaction mixture was heated at a temperature of about 100° C. for a period of about 4 hours. After this time the reaction mixture was filtered and additional sodium carbonate (5.0 grams) was added to the filtrate. The mixture was then vacuum distilled and the fraction boiling at 120° C. and 0.07 mm of Hg pressure was collected to yield the desired product N-(4-methyl-1,3-dioxolan-2-ylmethyl)-2-methoxyaniline.

후처리

  1. customequipped with a mechanical stirrer
  2. temperaturethermometer and reflux condenser
  3. filtrationAfter this time the reaction mixture was filtered
  4. additionadditional sodium carbonate (5.0 grams) was added to the filtrate
  5. distillationvacuum distilled
  6. customthe fraction boiling at 120° C. and 0.07 mm of Hg pressure was collected

출처 및 근거

ORD 기록
ord-e99f9d76b08a481ba3c31cb20e20a62f
출처 데이터셋
uspto-grants-1980_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04225335

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