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

HRID 601017

反応式

HRID 601017 の反応式
[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

参加物

4

反応物 2

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

生成物 1

HCID 28250194-Methoxy-6-nitro-1,3-benzodioxole収率 46%

試薬・触媒・溶媒 1

HCID 7918Acetic Anhydride溶媒

実験手順

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)

後処理

  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

出典と根拠

ORDレコード
ord-287c8eed20904c47bfb85e1d1d14d7e9
出典データセット
uspto-grants-2011_03
特許番号
US07902239B2

関連ノート

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