Potassium Iodide → N-[1-[2-(4-methoxyphenyl)ethyl]-4-piperidinyl]-2-benzothiazolamine

HRID 1085688

반응식

HRID 1085688 반응식
CS(O[CH2:6][CH2:7][C:8]1[CH:13]=[CH:12][C:11]([O:14][CH3:15])=[CH:10][CH:9]=1)(=O)=O.Br.Br.[NH:18]1[CH2:23][CH2:22][CH:21]([NH:24][C:25]2[S:26][C:27]3[CH:33]=[CH:32][CH:31]=[CH:30][C:28]=3[N:29]=2)[CH2:20][CH2:19]1.C(=O)([O-])[O-].[Na+].[Na+].[I-].[K+]>CN(C)C=O>[CH3:15][O:14][C:11]1[CH:10]=[CH:9][C:8]([CH2:7][CH2:6][N:18]2[CH2:19][CH2:20][CH:21]([NH:24][C:25]3[S:26][C:27]4[CH:33]=[CH:32][CH:31]=[CH:30][C:28]=4[N:29]=3)[CH2:22][CH2:23]2)=[CH:13][CH:12]=1

참가 물질

6

반응물 4

HCID 4875Potassium IodideHCID 10340Sodium CarbonateHCID 2779772-(4-Methoxyphenyl)ethyl methanesulfonateHCID 14575275HCID 14575275, 화합물

생성물 1

HCID 14575764N-[1-[2-(4-methoxyphenyl)ethyl]-4-piperidinyl]-2-benzothiazolamine수율 41%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
70 °C

실험 절차

A mixture of 2.3 parts of [2-(4-methoxyphenyl)ethyl] methanesulfonate, 4 parts of N-(4-piperidinyl)-2-benzothiazolamine dihydrobromide, 5.3 parts of sodium carbonate, 0.1 parts of potassium iodide and 90 parts of N,N-dimethylformamide was stirred overnight at 70° C. The reaction mixture was poured onto water and the product was extracted with methylbenzene. The extract was washed with water, dried, filtered and evaporated. The residue was crystallized from a mixture of 2-propanol and 2,2'-oxybispropane. The product was filtered off and dried, yielding 1.5 parts (41%) of N-[1-[2-(4-methoxyphenyl)-ethyl]-4-piperidinyl]-2-benzothiazolamine; mp. 142.5° C. (178).

후처리

  1. additionThe reaction mixture was poured onto water
  2. extractionthe product was extracted with methylbenzene
  3. washThe extract was washed with water
  4. customdried
  5. filtrationfiltered
  6. customevaporated
  7. customThe residue was crystallized from a mixture of 2-propanol and 2,2'-oxybispropane
  8. filtrationThe product was filtered off
  9. customdried

출처 및 근거

ORD 기록
ord-2b99b01b32df4e46b27ab0a7d10c157d
출처 데이터셋
uspto-grants-1991_04
특허 번호
US05010198

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