Acetonitrile → 1-Ethyl-N-methyl-N-pyridin-2-yl-1H-benzimidazol-2-amine

HRID 909855

反応式

HRID 909855 の反応式
N1C=CC=C[C:2]=1[CH2:7][NH:8][CH2:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][N:11]=1.[C:16](#[N:18])[CH3:17].[CH2:19]([N:21](CC)[CH2:22]C)C.C[C:27]([CH3:32])([CH3:31])C(Cl)=O>O>[CH2:7]([N:8]1[C:9]2[CH:10]=[CH:15][CH:14]=[CH:13][C:12]=2[N:11]=[C:19]1[N:21]([CH3:22])[C:32]1[CH:27]=[CH:31][CH:17]=[CH:16][N:18]=1)[CH3:2]

参加物

6

反応物 4

HCID 6342AcetonitrileHCID 8471TriethylamineHCID 62493Pivaloyl chlorideHCID 73759Bis(2-pyridylmethyl)amine

生成物 1

HCID 666282671-Ethyl-N-methyl-N-pyridin-2-yl-1H-benzimidazol-2-amine

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a flask were added 1.06 g of di-(2-picolyl)amine and 20 ml of acetonitrile. The solution was stirred under nitrogen, when 0.7 g of triethylamine were added, followed by 1.5 g of trimethylacetyl chloride. After 1 hour, 20 ml of water were added and the acetonitrile was removed. The product was extracted with ethyl acetate and washed with water. Following solvent removal, the product was recrystallized by dissolving in 6 ml hot hexane with 0.5 ml 2-propanol. Another 2 ml hexane were added and the mixture was cooled to 5 C, filtered, washed with hexane and dried, resulting in 1.3 g of an off-white solid.

後処理

  1. customthe acetonitrile was removed
  2. extractionThe product was extracted with ethyl acetate
  3. washwashed with water
  4. customFollowing solvent removal
  5. customthe product was recrystallized
  6. dissolutionby dissolving in 6 ml hot hexane with 0.5 ml 2-propanol
  7. additionAnother 2 ml hexane were added
  8. temperaturethe mixture was cooled to 5 C
  9. filtrationfiltered
  10. washwashed with hexane
  11. customdried

出典と根拠

ORDレコード
ord-c8b8a0e29bdf406c96a215cd5f5858f9
出典データセット
uspto-grants-2011_09
特許番号
US08018639B2

関連ノート

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