Nitric Acid → 4-Methoxy-6-nitro-1,3-benzodioxole

HRID 601017

반응식

HRID 601017 반응식
[CH3:1][O:2][C:3]1[C:11]2[O:10][CH2:9][O:8][C:7]=2[CH:6]=[CH:5][CH:4]=1.[N+:12]([O-])([OH:14])=[O:13]>C(OC(=O)C)(=O)C>[CH3:1][O:2][C:3]1[C:11]2[O:10][CH2:9][O:8][C:7]=2[CH:6]=[C:5]([N+:12]([O-:14])=[O:13])[CH:4]=1

참가 물질

4

반응물 2

HCID 944Nitric AcidHCID 5924784-Methoxybenzo[d][1,3]dioxole

생성물 1

HCID 28250194-Methoxy-6-nitro-1,3-benzodioxole수율 46%

시약·촉매·용매 1

HCID 7918Acetic Anhydride용매

실험 절차

4-Methoxy-benzo[1,3]dioxole (2.03 g, 13.34 mmole) was dissolved in acetic anhydride (20 mL) and cooled in an ice bath while stirring. Nitric acid (1.5 mL) was added dropwise with an addition funnel over 30 minutes. The ice bath was removed and the mixture was stirred overnight allowing the reaction to heat up to room temperature. The mixture was poured into ice water and the product crashed out and was filtered and washed with water. The precipitate was dried under vacuum in a dessicator yielding (1.21 g, 46% yield) of 4-methoxy-6-nitro-benzo[1,3]dioxole. NMR-DMSO-d6: 7.63 (s, 1H), 7.52 (s, 1H), 6.25 (s, 2H), 3.95 (s, 3H)

후처리

  1. temperaturecooled in an ice bath
  2. customThe ice bath was removed
  3. stirringthe mixture was stirred overnight
  4. customthe reaction
  5. filtrationwas filtered
  6. washwashed with water
  7. customThe precipitate was dried under vacuum in a dessicator

출처 및 근거

ORD 기록
ord-287c8eed20904c47bfb85e1d1d14d7e9
출처 데이터셋
uspto-grants-2011_03
특허 번호
US07902239B2

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