Sodium Carbonate → HCID 11610203, 화합물

HRID 2198784노트

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HRID 2198784 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 11610203HCID 11610203, 화합물

시약·촉매·용매 1

HCID 6395Methanesulfonic Acid용매

실험 절차

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:

후처리

  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

출처 및 근거

ORD 기록
ord-5da86096e18c4925afdbbf2613ed84f8
출처 데이터셋
uspto-grants-1982_11
특허 번호
US04359475

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