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Diisopropylethylamine → HCID 68727240, 화합물

HRID 408656
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HRID 408656 반응식
Cl[C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[C:9]([N+:12]([O-:14])=[O:13])[CH:10]=2)[N:5]=[C:4]([CH3:15])[CH:3]=1.[C:16]1([CH:22]2[CH2:26][CH2:25][NH:24][CH2:23]2)[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1.C(N(C(C)C)CC)(C)C>C(OCCO)C.O>[CH3:15][C:4]1[CH:3]=[C:2]([N:24]2[CH2:25][CH2:26][CH:22]([C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=3)[CH2:23]2)[C:11]2[C:6](=[CH:7][CH:8]=[C:9]([N+:12]([O-:14])=[O:13])[CH:10]=2)[N:5]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 81531DiisopropylethylamineHCID 31467433-PhenylpyrrolidineHCID 50849494-Chloro-2-methyl-6-nitroquinoline

생성물 1

HCID 68727240HCID 68727240, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 8076Glycol monoethyl ether용매

실험 절차

4-Chloro-2-methyl-6-nitroquinoline (0.2 g), 3-phenylpyrrolidine (0.14 g) and diisopropyl-ethylamine (0.27 mL) in 2-ethoxyethanol (4 mL) was heated in a microwave to 200° C. for 15 minutes. The reaction mixture was diluted with water and extracted with dichloromethane, washed with water, dried (Na2SO4), filtered and evaporated to give a yellow oil. The residue was purified by chromatography on silica, eluting with a mixture of dichloromethane, ethanol and ammonia (200:8:1). The desired fractions were concentrated to give the title compound as an orange oil.

후처리

  1. extractionextracted with dichloromethane
  2. washwashed with water
  3. dry with materialdried (Na2SO4)
  4. filtrationfiltered
  5. customevaporated
  6. customto give a yellow oil
  7. customThe residue was purified by chromatography on silica
  8. washeluting with a mixture of dichloromethane, ethanol and ammonia (200:8:1)
  9. concentrationThe desired fractions were concentrated

출처 및 근거

ORD 기록
ord-4ad53941504043fda5a49d00343054c2
출처 데이터셋
uspto-grants-2014_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08759348B2

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