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

HRID 6507

反応式

HRID 6507 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>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

5

反応物 2

HCID 944Nitric AcidHCID 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 washed 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. washthe reaction mixture was washed to room temperature
  4. additionThe solution was then poured into water
  5. filtrationthe precipitate was filtered off with suction
  6. washwashed with water
  7. customdried

出典と根拠

ORDレコード
ord-4f2ef7e7bc5d48b9b8a54d0213b449e8
出典データセット
uspto-grants-1993_09
特許番号
US05248823

関連ノート

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