Acetic Anhydride → N-(2H-1,3-Benzodioxol-5-yl)acetamide

HRID 1023322

반응식

HRID 1023322 반응식
[CH2:1]1[O:10][C:9]2[CH:8]=[CH:7][C:5]([NH2:6])=[CH:4][C:3]=2[O:2]1.[CH3:11][C:12](OC(C)=O)=[O:13].C([O-])(O)=O.[Na+]>CC(O)=O>[O:10]1[C:9]2[CH:8]=[CH:7][C:5]([NH:6][C:12](=[O:13])[CH3:11])=[CH:4][C:3]=2[O:2][CH2:1]1

참가 물질

5

반응물 3

HCID 7918Acetic AnhydrideHCID 843101,3-Benzodioxol-5-amineHCID 516892Sodium Bicarbonate

생성물 1

HCID 98688N-(2H-1,3-Benzodioxol-5-yl)acetamide수율 95%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

To a solution of 3,4-(Methylenedioxy)aniline (8 g, 58.3 mmol) in AcOH (120 ml) was added Ac2O (48 mL). The mixture was stirred for overnight. After reaction, the mixture was poured into saturated NaHCO3 solution, and then filtered. The filtrate was extracted with ethyl acetate to give N-(benzo[d][1,3]dioxol-5-yl)acetamide (10 g, 95%). LCMS: 180 [M+1]+; 1H NMR (DMSO-d6) δ 2.0 (s, 3H), 5.96 (s, 2H), 6.82 (d, 1H, J=8.1 Hz), 6.91 (d, 1H, J=2.1 Hz), 7.30 (d, 1H, J=1.8 Hz), 9.84 (s, 1H).

후처리

  1. customAfter reaction
  2. filtrationfiltered
  3. extractionThe filtrate was extracted with ethyl acetate

출처 및 근거

ORD 기록
ord-391fc02ba34c4fab8ce9b8b59709e8d8
출처 데이터셋
uspto-grants-2014_05
특허 번호
US08722703B2

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