Triethylamine → 4-Methylbenzimidazole

HRID 248836

반응식

HRID 248836 반응식
[NH2:1][C:2]1[C:7]([NH2:8])=[CH:6][CH:5]=[CH:4][C:3]=1[CH3:9].[CH2:10](N(CC)CC)C.COC(Cl)Cl>O1CCCC1>[CH3:9][C:3]1[C:2]2[N:1]=[CH:10][NH:8][C:7]=2[CH:6]=[CH:5][CH:4]=1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 175932,3-DiaminotolueneHCID 21004Methane, dichloromethoxy-

생성물 1

HCID 15193414-Methylbenzimidazole수율 100%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
0 °C

실험 절차

2,3 Diaminotoluene (675 mg, 5.53 mmol) was dissolved in 10 mL of dry tetrahydrofuran and triethylamine (0.77 mL, 5.53 mmol) was added. The mixture was cooled to 0° C. and 1,1-dichloromethyl methyl ether (0.50 mL, 5.53 mmol) was added and the reaction was allowed to warm to room temperature. After 20 hours, the reaction was quenched with sodium bicarbonate. The aqueous phase was extracted with ethyl acetate, dried over magnesium sulfate, filtered and the solvent removed to yield 730 mg (100%) of a brown solid.

후처리

  1. temperatureto warm to room temperature
  2. customthe reaction was quenched with sodium bicarbonate
  3. extractionThe aqueous phase was extracted with ethyl acetate
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered
  6. customthe solvent removed

출처 및 근거

ORD 기록
ord-db7a59d5b616435bbb5f75d38b4a5975
출처 데이터셋
uspto-grants-1993_05
특허 번호
US05212177

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