Potassium Iodide → 4,4-dimethyl-pyrazolidine N,N'-dicarboxylic acid di-tert-buty1 ester

HRID 36600

반응식

HRID 36600 반응식
[C:1]([O:5][C:6]([NH:8][NH:9][C:10]([O:12][C:13]([CH3:16])([CH3:15])[CH3:14])=[O:11])=[O:7])([CH3:4])([CH3:3])[CH3:2].C(=O)([O-])[O-].[K+].[K+].CS(O[CH2:28][C:29]([CH3:37])([CH3:36])[CH2:30]OS(C)(=O)=O)(=O)=O.[I-].[K+]>CN(C)C=O>[C:1]([O:5][C:6]([N:8]1[CH2:30][C:29]([CH3:37])([CH3:36])[CH2:28][N:9]1[C:10]([O:12][C:13]([CH3:16])([CH3:15])[CH3:14])=[O:11])=[O:7])([CH3:4])([CH3:3])[CH3:2]

참가 물질

6

반응물 4

HCID 4875Potassium IodideHCID 11430Potassium CarbonateHCID 85431Di-tert-butyl bicarbamateHCID 299203Neopentyl glycol dimethylsulfate

생성물 1

HCID 544895554,4-dimethyl-pyrazolidine N,N'-dicarboxylic acid di-tert-buty1 ester수율 2%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

41.8 g of hydrazine-N,N'-dicarboxylic acid di-tert-butyl ester, 74.5 g of potassium carbonate, 52.0 g of 2,2-dimethyl-1,3-propanediol dimethanesulfonate and 2.0 g of potassium iodide are stirred for 48 hours at 120°-130° C. in 360 ml of N,N-dimethylformamide. The reaction mixture is then concentrated; diethyl ether is added and the organic phase is washed with water. Mter drying over sodium sulfate, the reaction mixture is concentrated and purified by means of column chromatography to yield 1.1 g of the desired product, 4,4-dimethyl-pyrazolidine-N,N'-dicarboxylic acid di-tert-butyl ester, in the form of white crystals.

후처리

  1. concentrationThe reaction mixture is then concentrated
  2. additiondiethyl ether is added
  3. washthe organic phase is washed with water
  4. dry with materialMter drying over sodium sulfate
  5. concentrationthe reaction mixture is concentrated
  6. custompurified by means of column chromatography

출처 및 근거

ORD 기록
ord-d11c6c925c1348ed84d5539cdd66929d
출처 데이터셋
uspto-grants-1995_05
특허 번호
US05416065

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