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

HRID 1762812ノート

反応式

HRID 1762812 の反応式
[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]

参加物

8

反応物 5

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 962Water溶媒2 回HCID 6348Carbon Disulfide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-502666f2b2fd4074998404aa1ca6c6bb
出典データセット
uspto-grants-1989_05
特許番号
US04835153

反応ノート

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