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Diisopropylethylamine → HCID 68727240、化合物

HRID 408656
ノート
印刷プレビュー

反応式

HRID 408656 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

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

生成物 1

HCID 68727240HCID 68727240、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8076Glycol monoethyl ether溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-4ad53941504043fda5a49d00343054c2
出典データセット
uspto-grants-2014_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08759348B2

反応ノート

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