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

HRID 260584

반응식

HRID 260584 반응식
[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]

참가 물질

6

반응물 3

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

생성물 1

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

시약·촉매·용매 2

HCID 176Acetic Acid용매2회HCID 7918Acetic Anhydride용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-636c212bd395407ca76434af0ff340e6
출처 데이터셋
uspto-grants-1996_06
특허 번호
US05527945

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