Sodium Carbonate → HCID 11610203、化合物

HRID 2198784ノート

反応式

HRID 2198784 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][CH2:9][C:10](=O)[CH2:11][N:12]2[CH:16]=[CH:15][N:14]=[CH:13]2)=[CH:4][CH:3]=1.[CH2:18]([SH:21])[CH2:19][SH:20].C(=O)([O-])[O-].[Na+].[Na+]>CS(O)(=O)=O>[ClH:1].[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][CH2:9][C:10]2([CH2:11][N:12]3[CH:16]=[CH:15][N:14]=[CH:13]3)[S:21][CH2:18][CH2:19][S:20]2)=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 10340Sodium CarbonateHCID 109021,2-EthanedithiolHCID 110103354-(4-Chlorophenyl)-1-(imidazol-1-yl)butan-2-one

生成物 1

HCID 11610203HCID 11610203、化合物

試薬・触媒・溶媒 1

HCID 6395Methanesulfonic Acid溶媒

実験手順

A solution 1-[4-(4-chlorophenyl)butan-2-on-1-yl]imidazole (2.49 g) in 98% methanesulfonic acid (10 ml) was treated with ethane-1,2-dithiol (6 ml) and the mixture stirred overnight at room temperature. The resulting mixture was poured into excess aqueous sodium carbonate, extracted with ether (3×20 ml), the extracts washed, dried (MgSO4) and the ether evaporated. The residue was taken up in a small volume of ether and treated with ethereal hydrogen chloride until precipitation was complete. The resulting precipitate was filtered off and recrystallized from methanol/ethyl acetate, to give 1-[[2-(2-(4-chlorophenyl)ethyl)-1,3-dithiolan-2-yl]methyl]imidazole hydrochloride, m.p. 206.5°-208° C. Similarly proceeding as above, but substituting the appropriate ethan-1,2-dithiol and the appropriate ketone as exemplified in Preparations 1, 2, 3 or 4 in place of 1-[4-(4-chlorophenyl)butan-2-on-1-yl]imidazole there may be prepared, for example, the following compounds:

後処理

  1. extractionextracted with ether (3×20 ml)
  2. washthe extracts washed
  3. dry with materialdried (MgSO4)
  4. customthe ether evaporated
  5. additiontreated with ethereal hydrogen chloride until precipitation
  6. filtrationThe resulting precipitate was filtered off
  7. customrecrystallized from methanol/ethyl acetate

出典と根拠

ORDレコード
ord-5da86096e18c4925afdbbf2613ed84f8
出典データセット
uspto-grants-1982_11
特許番号
US04359475

反応ノート

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