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Potassium Iodide → HCID 20288043, 화합물

HRID 126872
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HRID 126872 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.[CH3:15][O:16][C:17]1[CH:22]=[CH:21][C:20]([C:23](=[O:31])[CH2:24][CH:25]2[CH2:30][CH2:29][NH:28][CH2:27][CH2:26]2)=[CH:19][CH:18]=1.C(=O)([O-])[O-].[Na+].[Na+].[I-].[K+]>CC(C)CC(=O)C>[CH3:15][O:16][C:17]1[CH:22]=[CH:21][C:20]([C:23](=[O:31])[CH2:24][CH:25]2[CH2:26][CH2:27][N:28]([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])[CH2:29][CH2:30]2)=[CH:19][CH:18]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 4875Potassium IodideHCID 10340Sodium CarbonateHCID 36534711-(2-chloroethyl)-1H-benzo[d]imidazol-2(3H)-oneHCID 20288060HCID 20288060, 화합물

생성물 1

HCID 20288043HCID 20288043, 화합물수율 36.5%

시약·촉매·용매 1

HCID 7909
Methyl Isobutyl Ketone
용매

실험 절차

A mixture of 3.92 parts of 1-(2-chloroethyl)-1,3-dihydro-2H-benzimidazol-2-one, 5.4 parts of 1-(4-methoxyphenyl)-2-(4-piperidinyl)ethanone hydrochloride, 5.3 parts of sodium carbonate, 0.1 parts of potassium iodide and 200 parts of 4-methyl-2-pentanone is distilled azeotropically to dry overnight. After cooling, the precipitated product is filtered off, washed with water and dissolved in trichloromethane. The latter is dried, filtered and evaporated. The residue is crystallized from 2-propanol, yielding 2.9 parts (36.5%) of 1,3-dihydro-1-[2-[4-[2-(4-methoxyphenyl)-2-oxoethyl]-1-piperidinyl]ethyl]-2H-benzimidazol-2-one; mp. 155.9° C.

후처리

  1. distillationis distilled azeotropically
  2. customto dry overnight
  3. temperatureAfter cooling
  4. filtrationthe precipitated product is filtered off
  5. washwashed with water
  6. dissolutiondissolved in trichloromethane
  7. customThe latter is dried
  8. filtrationfiltered
  9. customevaporated
  10. customThe residue is crystallized from 2-propanol

출처 및 근거

ORD 기록
ord-7f6c6cf8037c40eaa3c1deeabc217f1b
출처 데이터셋
uspto-grants-1981_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04254127

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