Nitric Acid → 1,1,4,4-Tetramethyl-6-nitro-1,2,3,4-tetrahydronaphthalene

HRID 260584

反応式

HRID 260584 の反応式
[N+:1]([O-:4])(O)=[O:2].[CH3:5][C:6]1([CH3:18])[C:15]2[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=2)[C:9]([CH3:17])([CH3:16])[CH2:8][CH2:7]1.O>C(O)(=O)C.C(OC(=O)C)(=O)C>[N+:1]([C:13]1[CH:12]=[CH:11][C:10]2[C:9]([CH3:17])([CH3:16])[CH2:8][CH2:7][C:6]([CH3:18])([CH3:5])[C:15]=2[CH:14]=1)([O-:4])=[O:2]

参加物

6

反応物 3

HCID 944Nitric AcidHCID 962WaterHCID 811861,1,4,4-Tetramethyltetralin

生成物 1

HCID 139871261,1,4,4-Tetramethyl-6-nitro-1,2,3,4-tetrahydronaphthalene

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒2 回HCID 7918Acetic Anhydride溶媒

実験手順

77.2 ml of glacial acetic acid and 20.8 ml of nitric acid (98% strength) were mixed while cooling and then added dropwise within 2 hours to a solution of 65.8 g (0.35 mol) of 1,2,3,4-tetrahydro-1,1,4,4-tetramethylnaphthalene in 154 ml of glacial acetic acid and 257 ml of acetic anhydride in a salt/ice bath. After the addition was complete, the reaction mixture was warmed to room temperature and stirred overnight. The solution was then poured into water, and the precipitate was filtered off with suction, washed with water and dried. 79.7 g of crude 2-nitro-5,6,7,8-tetrahydro-5,5,8,8-tetramethylnaphthalene of melting point 46°-50° C. were obtained.

後処理

  1. temperaturewhile cooling
  2. additionAfter the addition
  3. filtrationthe precipitate was filtered off with suction
  4. washwashed with water
  5. customdried

出典と根拠

ORDレコード
ord-636c212bd395407ca76434af0ff340e6
出典データセット
uspto-grants-1996_06
特許番号
US05527945

関連ノート

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