Pyridine → HCID 18403464、化合物

HRID 1017210ノート

反応式

HRID 1017210 の反応式
[N+:1]([C:4]1[CH:13]=[CH:12][C:7]([O:8][CH2:9][CH2:10][NH2:11])=[CH:6][CH:5]=1)([O-:3])=[O:2].N1C=CC=CC=1.[C:20](Cl)(=[O:24])[CH:21]([CH3:23])[CH3:22]>C(Cl)Cl.Cl>[N+:1]([C:4]1[CH:13]=[CH:12][C:7]([O:8][CH2:9][CH2:10][NH:11][C:20](=[O:24])[CH:21]([CH3:23])[CH3:22])=[CH:6][CH:5]=1)([O-:3])=[O:2]

参加物

6

反応物 3

HCID 1049PyridineHCID 62325Isobutyryl chlorideHCID 122944662-(4-Nitrophenoxy)ethanamine

生成物 1

HCID 18403464HCID 18403464、化合物

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒HCID 6344Dichloromethane溶媒

実験手順

2-(4-Nitro-phenoxy)ethylamine (0.27 g) was dissolved in dry DCM (8.5 ml) and dry pyridine (0.15 ml) and isobutyryl chloride (0.12 ml) were then added. After stirring for 1 h at room temperature, the reaction mixture was then diluted with HCl 3 N (50 ml) and extracted with ethyl acetate (50 ml), then the organic phase was washed with brine (50 ml). The organic layer was separated, dried, filtered and evaporated under vacuum to give a crude product which was crystallized (diethyl ether, 7 ml) to give the title compound (0.11 g) as a yellow solid. m.p. 102-103°.

後処理

  1. extractionextracted with ethyl acetate (50 ml)
  2. washthe organic phase was washed with brine (50 ml)
  3. customThe organic layer was separated
  4. customdried
  5. filtrationfiltered
  6. customevaporated under vacuum
  7. customto give a crude product which
  8. customwas crystallized (diethyl ether, 7 ml)

出典と根拠

ORDレコード
ord-a3979d4e05dc4badb73fa6fce8d45f95
出典データセット
uspto-grants-2002_11
特許番号
US06479488B1

反応ノート

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