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Toluene → Methyl 1,2-dimethyl-1H-benzo[d]imidazole-5-carboxylate

HRID 928446
ノート
印刷プレビュー

反応式

HRID 928446 の反応式
[CH3:1][N:2]1[C:6]2[CH:7]=[CH:8][C:9]([C:11]([OH:13])=[O:12])=[CH:10][C:5]=2[N:4]=[C:3]1[CH3:14].[C:15]1(C)C=CC=CC=1>CO>[CH3:1][N:2]1[C:6]2[CH:7]=[CH:8][C:9]([C:11]([O:13][CH3:15])=[O:12])=[CH:10][C:5]=2[N:4]=[C:3]1[CH3:14]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 1140TolueneHCID 8452601,2-dimethyl-1H-1,3-benzodiazole-5-carboxylic acid

生成物 1

HCID 21998749Methyl 1,2-dimethyl-1H-benzo[d]imidazole-5-carboxylate

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a suspension of 1,2-Dimethyl-1H-benzo[d]imidazole-5-carboxylic acid (crude, 2.54 g, approx. 9.35 mmol) in MeOH (15.5 ml)/toluene (78 ml) Trimethylsilyldiazomethane (2 M solution in hexane, 7.0 ml, 14 mmol) was added at 0-10° C. The reaction mixture was stirred at it for 1 hour. The reaction mixture was evaporated under reduced pressure. The residue was taken up in DCM, Remaining insoluble solid was filtered off. The filtrate was evaporated again to dryness to afford crude Methyl 1,2-dimethyl-1H-benzo[d]imidazole-5-carboxylate

後処理

  1. additionwas added at 0-10° C
  2. customThe reaction mixture was evaporated under reduced pressure
  3. filtrationwas filtered off
  4. customThe filtrate was evaporated again to dryness

出典と根拠

ORDレコード
ord-e526c639768d4100a852bb5e94a042d8
出典データセット
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09290485B2

反応ノート

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