Triethylamine → 4-Methylbenzimidazole

HRID 248836

反応式

HRID 248836 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 15193414-Methylbenzimidazole収率 100%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
0 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-db7a59d5b616435bbb5f75d38b4a5975
出典データセット
uspto-grants-1993_05
特許番号
US05212177

関連ノート

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