Methanesulfonic Acid → 2-(Benzotriazol-2-yl)-4-methyl-6-tetracosylphenol

HRID 279964

반응식

HRID 279964 반응식
[OH:1][C:2]1[CH:7]=[CH:6][C:5]([CH3:8])=[CH:4][C:3]=1[N:9]1[N:13]=[C:12]2[CH:14]=[CH:15][CH:16]=[CH:17][C:11]2=[N:10]1.CS(O)(=O)=O.[CH2:23]=[CH:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH3:34]>>[OH:1][C:2]1[C:7]([CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:34][CH2:33][CH2:32][CH2:31][CH2:30][CH2:29][CH2:28][CH2:27][CH2:26][CH2:25][CH2:24][CH3:23])=[CH:6][C:5]([CH3:8])=[CH:4][C:3]=1[N:9]1[N:13]=[C:12]2[CH:14]=[CH:15][CH:16]=[CH:17][C:11]2=[N:10]1

참가 물질

4

반응물 3

HCID 6395Methanesulfonic AcidHCID 81831-DodeceneHCID 17113Drometrizole

생성물 1

HCID 201956522-(Benzotriazol-2-yl)-4-methyl-6-tetracosylphenol

반응 조건

온도
160 °C

실험 절차

Using the general procedure of Example 1, 112 grams of 2-(2-hydroxy-5-methylphenyl)-2H-benzotriazole, 33 ml of methanesulfonic acid and 444 ml (2 moles) of a mixture of tetracosenes (prepared by the dimerization of n-dodecene) are heated at 160° C.; for 96 hours. The reaction mixture is cooled and the product isolated by the general procedure described in Example 1. The excess hydrocarbons are removed by distillation at 190° C./0.04 mm. The above-named product is obtained in a yield of 103.6 grams as a yellow liquid. The liquid still contained inert hydrocarbon diluents which are removed by flash chromatography using silica gel and heptane/toluene 75/25 to give a pure product in a yield of 15 grams as a yellow liquid.

후처리

  1. temperatureThe reaction mixture is cooled
  2. customthe product isolated by the general procedure
  3. customThe excess hydrocarbons are removed by distillation at 190° C./0.04 mm
  4. customThe above-named product is obtained in a yield of 103.6 grams as a yellow liquid
  5. customThe liquid still contained inert hydrocarbon diluents which are removed by flash chromatography
  6. customto give a pure product in a yield of 15 grams as a yellow liquid

출처 및 근거

ORD 기록
ord-ae67741882134cd8b4d5e3a96edbcd95
출처 데이터셋
uspto-grants-1986_05
특허 번호
US04587346

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