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

HRID 635272ノート

反応式

HRID 635272 の反応式
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

参加物

9

反応物 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

生成物 1

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

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒HCID 8471Triethylamine溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-bf5ce4330df84541bd33667931603c63
出典データセット
uspto-grants-2001_02
特許番号
US06187774B1

反応ノート

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