Potassium Hydroxide → Diisopropyl(2,5-diisopropyl-2,5-diaza-7,9-dithiabicyclo-[4,3,0]-nonane-8-ylidene)malonate

HRID 1762812노트

반응식

HRID 1762812 반응식
[S:1](=O)(O)[O-].[Na+].[CH:6]([CH:8]=O)=O.[CH:10]([NH:13][CH2:14][CH2:15][NH:16][CH:17]([CH3:19])[CH3:18])([CH3:12])[CH3:11].[S:20]1[CH:24]=CC(C([O-])=O)S1.[C:28]([O:37][CH:38]([CH3:40])[CH3:39])(=[O:36])[CH2:29][C:30]([O:32][CH:33]([CH3:35])[CH3:34])=[O:31].[OH-].[K+]>O.C(=S)=S>[CH:38]([O:37][C:28](=[O:36])[C:29](=[C:24]1[S:20][CH:15]2[CH:14]([N:13]([CH:10]([CH3:12])[CH3:11])[CH2:6][CH2:8][N:16]2[CH:17]([CH3:19])[CH3:18])[S:1]1)[C:30]([O:32][CH:33]([CH3:34])[CH3:35])=[O:31])([CH3:40])[CH3:39]

참가 물질

8

반응물 5

HCID 14797Potassium HydroxideHCID 77628N,N'-DiisopropylethylenediamineHCID 83223Diisopropyl malonateHCID 23706077Sodium;hydrogen sulfite;oxaldehydeHCID 86638310Dithiolate

생성물 1

HCID 15623889Diisopropyl(2,5-diisopropyl-2,5-diaza-7,9-dithiabicyclo-[4,3,0]-nonane-8-ylidene)malonate수율 45%

시약·촉매·용매 2

HCID 962Water용매2회HCID 6348Carbon Disulfide용매

실험 절차

To a suspension of 1.7 g of glyoxal sodium bisulfite in 12 ml of water was added N,N'-diisopropylethylenediamine dropwise at room temperature and the mixture was stirred until it became a homogeneous solution. To this solution was added dropwise at 0° C. the dithiolate solution which had been prepared previously by the reaction of 1.13 g of diisopropyl malonate with 0.55 g of carbon disulfide in the presence of 2.9 g of 30% aqueous potassium hydroxide. After the mixture was stirred for additional 30 minutes, 50 ml of water was added to the reaction solution. The solid deposited was collected by filtration and recrystalized from ethyl acetate-n-hexane to give 1.16 g of the desired product.

후처리

  1. stirringAfter the mixture was stirred for additional 30 minutes
  2. filtrationThe solid deposited was collected by filtration
  3. customrecrystalized from ethyl acetate-n-hexane

출처 및 근거

ORD 기록
ord-502666f2b2fd4074998404aa1ca6c6bb
출처 데이터셋
uspto-grants-1989_05
특허 번호
US04835153

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