Potassium Carbonate → HCID 57036075、化合物

HRID 2260806

反応式

HRID 2260806 の反応式
Cl[C:2]1[S:6][N:5]=[C:4]([CH3:7])[N:3]=1.[CH3:8][N:9]1[CH2:14][C@@H:13]2[CH2:15][C@H:10]1[CH2:11][NH:12]2.C(=O)([O-])[O-].[K+].[K+]>O1CCCC1.C(Cl)Cl>[CH3:8][N:9]1[CH2:14][C@@H:13]2[CH2:15][C@H:10]1[CH2:11][N:12]2[C:2]1[S:6][N:5]=[C:4]([CH3:7])[N:3]=1

参加物

6

反応物 3

HCID 11430Potassium CarbonateHCID 11029795(1S,4S)-2-Methyl-2,5-diazabicyclo[2.2.1]heptaneHCID 129191595-Chloro-3-methyl-1,2,4-thiadiazole

生成物 1

HCID 57036075HCID 57036075、化合物収率 36.2%

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 8028Tetrahydrofuran溶媒2 回

実験手順

A solution of 1.04 g of 5-chloro-3-methyl-1,2,4-thiadiazole, prepared by the procedure of J. Goerdeler, Chim. Ber., 1957, 90, 182, in 2 ml of tetrahydrofuran is added over one hour to a solution of 0.825 g of (S,S)-2-methyl-2,5-diazabicyclo[2.2.1]heptane and 0.77 g of potassium carbonate in 10 ml of tetrahydrofuran. The reaction mixture is stirred at room temperature overnight, diluted with methylene chloride and the organic layer is washed with water. The methylene chloride solution is dried and concentrated in vacuo to dryness. The residue is purified by chromatography (aluminum oxide, Activity Grade 2.5: 2% methyl alcohol/methylene chloride) to give 0.56 g of the desired product:

後処理

  1. washthe organic layer is washed with water
  2. dry with materialThe methylene chloride solution is dried
  3. concentrationconcentrated in vacuo to dryness
  4. customThe residue is purified by chromatography (aluminum oxide, Activity Grade 2.5: 2% methyl alcohol/methylene chloride)

出典と根拠

ORDレコード
ord-8cf852a12857412ebe9b93cbfd6a1649
出典データセット
uspto-grants-1995_12
特許番号
US05478939

関連ノート

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