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Cyanuric chloride → HCID 20272144, 화합물

HRID 484938
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HRID 484938 반응식
[N:1]1[C:8](Cl)=[N:7][C:5](Cl)=[N:4][C:2]=1[Cl:3].[CH2:10]([CH:12]([CH2:25][CH2:26][CH2:27][CH3:28])[CH2:13][NH:14][CH:15]1[CH2:20][C:19]([CH3:22])([CH3:21])[NH:18][C:17]([CH3:24])([CH3:23])[CH2:16]1)[CH3:11].[OH-].[Na+]>CC(C)=O.O>[Cl:3][C:2]1[N:1]=[C:8]([N:14]([CH2:13][CH:12]([CH2:10][CH3:11])[CH2:25][CH2:26][CH2:27][CH3:28])[CH:15]2[CH2:16][C:17]([CH3:24])([CH3:23])[NH:18][C:19]([CH3:21])([CH3:22])[CH2:20]2)[N:7]=[C:5]([N:14]([CH:15]2[CH2:16][C:17]([CH3:24])([CH3:23])[NH:18][C:19]([CH3:21])([CH3:22])[CH2:20]2)[CH2:13][CH:12]([CH2:10][CH3:11])[CH2:25][CH2:26][CH2:27][CH3:28])[N:4]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 7954Cyanuric chlorideHCID 14798Sodium HydroxideHCID 20272156N-(2-Ethylhexyl)-2,2,6,6-tetramethyl-4-piperidinamine

생성물 1

HCID 20272144HCID 20272144, 화합물

시약·촉매·용매 2

HCID 180Acetone용매2회HCID 962Water용매2회

실험 절차

A suspension of 9.2 g of cyanuric chloride in 60 ml of acetone and 20 ml of water was added dropwise, with stirring, at 20°-25° C. to a solution of 29.5 g of 4-(2-ethylhexylamino)-2,2,6,6-tetramethylpiperidine in 50 ml of acetone, after which a solution of 4.2 g of sodium hydroxide in 20 ml of water was added to the mixture. The resulting reaction mixture was then stirred for 4 hours at 45°-50° C. At the end of this time, the acetone was distilled off and the oily residue was extracted with ethyl acetate. The extract was dried over anhydrous potassium carbonate, and the ethyl acetate was distilled off. The resulting oil was purified by column chromatography through silica gel, eluted with a 4:1 by volume mixture of hexane and ethyl acetate, to give the title compound as a colourless oil. The Rf value of this compound on thin layer chromatography was 0.62, using silica gel and using, as developing solvent, a 4:1:0.4 by volume mixture of ethyl acetate, methanol and triethylamine.

후처리

  1. additionwas added dropwise
  2. customThe resulting reaction mixture
  3. distillationAt the end of this time, the acetone was distilled off
  4. extractionthe oily residue was extracted with ethyl acetate
  5. dry with materialThe extract was dried over anhydrous potassium carbonate
  6. distillationthe ethyl acetate was distilled off
  7. customThe resulting oil was purified by column chromatography through silica gel
  8. washeluted with a 4:1 by volume mixture of hexane and ethyl acetate

출처 및 근거

ORD 기록
ord-2eb00fd8531c4b0196c3104b697cc214
출처 데이터셋
uspto-grants-1985_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04533688

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