Potassium Carbonate → 8-methyl-3,4-dihydro-2H-[1,3]thiazino[3,2-a]benzimidazole

HRID 1471239ノート

反応式

HRID 1471239 の反応式
[SH:1][C:2]1[NH:3][C:4]2[CH:10]=[C:9]([CH3:11])[CH:8]=[CH:7][C:5]=2[N:6]=1.C(=O)([O-])[O-].[K+].[K+].I[CH2:19][CH2:20][CH2:21]I>CN(C)C=O>[CH3:11][C:9]1[CH:8]=[CH:7][C:5]2[N:6]3[CH2:21][CH2:20][CH2:19][S:1][C:2]3=[N:3][C:4]=2[CH:10]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 123141,3-DiiodopropaneHCID 178423448HCID 178423448、化合物

生成物 1

HCID 666281468-methyl-3,4-dihydro-2H-[1,3]thiazino[3,2-a]benzimidazole収率 25.3%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a flask were added 2 g 2-mercapto-5-methylbenzimidazole, 4.2 g potassium carbonate, 4.0 g 1,3-diiodopropane and 60 ml N,N-dimethylformamide. The mixture was heated to 50 C under nitrogen for 5 hours and then cooled to 22 C. The reaction was quenched with 100 ml water and the product was extracted twice with ethyl acetate and washed twice with water. Following removal of the solvent, the product was recrystallized by dissolving in a hot mixture of 50 ml hexane with 10 ml 2-propanol. After cooling to 5 C, the product was filtered, washed with hexane and dried giving 0.63 g of an off-white solid.

後処理

  1. temperatureThe mixture was heated to 50 C under nitrogen for 5 hours
  2. temperaturecooled to 22 C
  3. customThe reaction was quenched with 100 ml water
  4. extractionthe product was extracted twice with ethyl acetate
  5. washwashed twice with water
  6. customremoval of the solvent
  7. customthe product was recrystallized
  8. dissolutionby dissolving in a hot mixture of 50 ml hexane with 10 ml 2-propanol
  9. temperatureAfter cooling to 5 C
  10. filtrationthe product was filtered
  11. washwashed with hexane
  12. customdried

出典と根拠

ORDレコード
ord-45b0c59fdbe444ecbd3a79629f012738
出典データセット
uspto-grants-2015_04
特許番号
US09011734B2

反応ノート

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