Potassium Iodide → HCID 20288037、化合物

HRID 126870ノート

反応式

HRID 126870 の反応式
Cl[CH2:2][CH2:3][N:4]1[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[NH:6][C:5]1=[O:13].Cl.[F:15][C:16]1[CH:21]=[CH:20][C:19]([C:22](=[O:30])[CH2:23][CH:24]2[CH2:29][CH2:28][NH:27][CH2:26][CH2:25]2)=[CH:18][CH:17]=1.C(=O)([O-])[O-].[Na+].[Na+].[I-].[K+]>O.CC(C)CC(=O)C>[F:15][C:16]1[CH:21]=[CH:20][C:19]([C:22](=[O:30])[CH2:23][CH:24]2[CH2:29][CH2:28][N:27]([CH2:2][CH2:3][N:4]3[C:8]4[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=4[NH:6][C:5]3=[O:13])[CH2:26][CH2:25]2)=[CH:18][CH:17]=1

参加物

7

反応物 4

HCID 4875Potassium IodideHCID 10340Sodium CarbonateHCID 36534711-(2-chloroethyl)-1H-benzo[d]imidazol-2(3H)-oneHCID 20288069HCID 20288069、化合物

生成物 1

HCID 20288037HCID 20288037、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒2 回HCID 7909Methyl Isobutyl Ketone溶媒

実験手順

A mixture of 2.16 parts of 1-(2-chloroethyl)-1,3-dihydro-2H-benzimidazol-2-one, 2.57 parts of 1-(4-fluorophenyl)-2-(4-piperidinyl)ethanone hydrochloride, 5.3 parts of sodium carbonate, 0.2 parts of potassium iodide and 200 parts of 4-methyl-2-pentanone is stirred and refluxed for 15 hours using a water-separator. The reaction mixture is cooled, water is added and the layers are separated. The organic phase is dried, filtered and evaporated. The residue is crystallized from a mixture of 2,2'-oxybispropane and 2-propanol. The product is filtered off and dried, yielding 2.5 parts of 1-[2-[4-[2-(4-fluorophenyl)-2-oxoethyl]-1-piperidinyl]ethyl]-1,3-dihydro-2H-benzimidazol-2-one; mp. 180.6° C.

後処理

  1. temperaturerefluxed for 15 hours
  2. temperatureThe reaction mixture is cooled
  3. customthe layers are separated
  4. customThe organic phase is dried
  5. filtrationfiltered
  6. customevaporated
  7. customThe residue is crystallized from a mixture of 2,2'-oxybispropane and 2-propanol
  8. filtrationThe product is filtered off
  9. customdried

出典と根拠

ORDレコード
ord-173e6664430d41d9ae34feea31fb7027
出典データセット
uspto-grants-1981_03
特許番号
US04254127

反応ノート

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