Potassium Iodide → 3-(3-(4-benzylpiperidin-1-yl)propyl)-6,7,8,9-tetrahydro-5H-1,2,4-triazolo[4,3-a]azepine

HRID 635272노트

반응식

HRID 635272 반응식
CS(Cl)(=O)=O.O[CH2:7][CH2:8][CH2:9][C:10]1[N:14]2[CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][C:13]2=[N:12][N:11]=1.[CH2:20]([CH:27]1[CH2:32][CH2:31][NH:30][CH2:29][CH2:28]1)[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1.C(=O)([O-])[O-].[K+].[K+].[I-].[K+]>CN(C)C=O.O.C(N(CC)CC)C>[CH2:20]([CH:27]1[CH2:32][CH2:31][N:30]([CH2:7][CH2:8][CH2:9][C:10]2[N:14]3[CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][C:13]3=[N:12][N:11]=2)[CH2:29][CH2:28]1)[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1

참가 물질

9

반응물 5

HCID 4875Potassium IodideHCID 11430Potassium CarbonateHCID 31297Methanesulfonyl chlorideHCID 317384-BenzylpiperidineHCID 246884223-(3-hydroxypropyl)-6,7,8,9-tetrahydro-5H-1,2,4-triazolo[4,3-a]azepine

생성물 1

HCID 155211573-(3-(4-benzylpiperidin-1-yl)propyl)-6,7,8,9-tetrahydro-5H-1,2,4-triazolo[4,3-a]azepine

시약·촉매·용매 3

HCID 962Water용매HCID 6228Dimethylformamide용매HCID 8471Triethylamine용매

실험 절차

Triethylamine (1.4 ml) and methanesulfonyl chloride (0.62 ml) were added to a solution of 3-(3-hydroxypropyl)-6,7,8,9-tetrahydro-5H-1,2,4-triazolo[4,3-a]azepine (0.98 g) obtained in the same manner as in Example 4 in dimethylformamide (20 ml) with stirring. Then, 4-benzylpiperidine (0.88 g), potassium carbonate (1.38 g) and potassium iodide (0.83 g) were added and the mixture was stirred for 4 hours at 60° C. After the completion of the reaction, the reaction mixture was poured into water, extracted with ethyl acetate, washed with water, and dried over magnesium sulfate. The solution was concentrated under reduced pressure to give 3-(3-(4-benzylpiperidin-1-yl)propyl)-6,7,8,9-tetrahydro-5H-1,2,4-triazolo[4,3-a]azepine.

후처리

  1. stirringthe mixture was stirred for 4 hours at 60° C
  2. customAfter the completion of the reaction
  3. extractionextracted with ethyl acetate
  4. washwashed with water
  5. dry with materialdried over magnesium sulfate
  6. concentrationThe solution was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-bf5ce4330df84541bd33667931603c63
출처 데이터셋
uspto-grants-2001_02
특허 번호
US06187774B1

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