Potassium Iodide → HCID 20288037, 화합물

HRID 126870노트

반응식

HRID 126870 반응식
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

참가 물질

7

반응물 4

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

생성물 1

HCID 20288037HCID 20288037, 화합물

시약·촉매·용매 2

HCID 962Water용매2회HCID 7909Methyl Isobutyl Ketone용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-173e6664430d41d9ae34feea31fb7027
출처 데이터셋
uspto-grants-1981_03
특허 번호
US04254127

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