Potassium Carbonate → HCID 57036075, 화합물

HRID 2260806

반응식

HRID 2260806 반응식
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

참가 물질

6

반응물 3

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

생성물 1

HCID 57036075HCID 57036075, 화합물수율 36.2%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 8028Tetrahydrofuran용매2회

실험 절차

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:

후처리

  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)

출처 및 근거

ORD 기록
ord-8cf852a12857412ebe9b93cbfd6a1649
출처 데이터셋
uspto-grants-1995_12
특허 번호
US05478939

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