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Triethylamine → HCID 21266099, 화합물

HRID 566317
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HRID 566317 반응식
[NH:1]([CH:3]([CH2:7][CH2:8][CH2:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)[CH:4]([OH:6])[CH3:5])[NH2:2].C(N(CC)CC)C.[CH3:23][O:24][C:25](OC)=[C:26]([C:29]#[N:30])[C:27]#[N:28]>CO.C(O)(=O)CC(CC(O)=O)(C(O)=O)O.C(OCC)(=O)C>[NH2:30][C:29]1[N:1]([CH:3]([CH2:7][CH2:8][CH2:9][C:10]2[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=2)[CH:4]([OH:6])[CH3:5])[N:2]=[C:25]([O:24][CH3:23])[C:26]=1[C:27]#[N:28]
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참가 물질

7

반응물 3

HCID 8471TriethylamineHCID 110079702-(dimethoxymethylidene)propanedinitrileHCID 21266058HCID 21266058, 화합물

생성물 1

HCID 21266099HCID 21266099, 화합물수율 30.5%

시약·촉매·용매 3

HCID 311Citric Acid용매HCID 887Methanol용매
HCID 8857
Ethyl Acetate
용매

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온도
20 °C

실험 절차

4.2 g of 3-hydrazino-2-hydroxy-6-phenylhexane are are dissolved in 20 ml of methanol, and 1.38 ml of triethylamine are added. Then, 1.38 g of 1,1-dimethoxy-2,2-dicyano-ethylene are added. The reaction solution is stirred for 2 hours at approx. 20° C. For work-up, the mixture is diluted with citric acid solution and ethyl acetate and extracted three times with ethyl acetate. The combined ethyl acetate phases are dried with magnesium sulphate and evaporated in vacuo. The evaporation residue is chromatographed on silica gel (Merck Si 60 0.04-0.063 mm) with a cyclohexane/ethyl acetate mixture in a ratio of 4:1 to 1:1. This gives a fraction which, after evaporation in vacuo, affords 0.959 g (=30.5% of theory) of 5-amino-4-cyano-3-methoxy-1-[2-hydroxy-6-phenyl-hex-3-yl]-pyrazole as diastereomer mixture.

후처리

  1. extractionextracted three times with ethyl acetate
  2. dry with materialThe combined ethyl acetate phases are dried with magnesium sulphate
  3. customevaporated in vacuo
  4. customThe evaporation residue is chromatographed on silica gel (Merck Si 60 0.04-0.063 mm) with a cyclohexane/ethyl acetate mixture in a ratio of 4:1 to 1:1
  5. customThis gives a fraction which
  6. customafter evaporation in vacuo

출처 및 근거

ORD 기록
ord-e64f29c49e8a4be69f9fc2976bb6b3f7
출처 데이터셋
uspto-grants-2001_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06174884B1

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