Acetic Acid → 5-Methoxy-2,3,3-trimethyl-3H-indole

HRID 127152

반응식

HRID 127152 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([NH2:9])=[CH:5][CH:4]=1.[CH3:10][C:11](O)([C:13](=O)[CH3:14])[CH3:12].C(O)(=O)C.C1(C)C=CC=CC=1>O>[CH3:14][C:13]1[C:11]([CH3:12])([CH3:10])[C:5]2[CH:4]=[C:3]([O:2][CH3:1])[CH:8]=[CH:7][C:6]=2[N:9]=1

참가 물질

6

반응물 4

HCID 176Acetic AcidHCID 1140TolueneHCID 7732P-AnisidineHCID 82613-Hydroxy-3-methyl-2-butanone

생성물 1

HCID 110953925-Methoxy-2,3,3-trimethyl-3H-indole

시약·촉매·용매 1

HCID 962Water용매2회

반응 조건

온도
220 °C

실험 절차

246 parts of p-anisidine, 204 parts of 2-methyl-2-hydroxy-butan-3-one and 10 parts of acetic acid in 650 parts of toluene are heated, with removal of water from the system, until no more water separates off. The solvent is then distilled off and the residue is heated for 5 hours at 220° C. After cooling to 160° C., 10 parts of concentrated sulfuric acid are added; the mixture is kept at 160° C. for 3 hours, whilst distilling off the water formed. Distillation under reduced pressure (21 mbar) gives 318.7 parts of 5-methoxy-2,3,3-trimethyl-indolenine (melting point 53°-54° C.), corresponding to 84.3% of theory.

후처리

  1. distillationThe solvent is then distilled off
  2. temperatureAfter cooling to 160° C.
  3. addition10 parts of concentrated sulfuric acid are added
  4. distillationwhilst distilling off the water
  5. customformed
  6. distillationDistillation under reduced pressure (21 mbar)

출처 및 근거

ORD 기록
ord-7f18f49789c24e61a207293027d2f17d
출처 데이터셋
uspto-grants-1981_03
특허 번호
US04255333

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