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

HRID 36600ノート

反応式

HRID 36600 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-d11c6c925c1348ed84d5539cdd66929d
出典データセット
uspto-grants-1995_05
特許番号
US05416065

反応ノート

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