4-Chloroaniline → HCID 15086593、化合物

HRID 359081ノート

反応式

HRID 359081 の反応式
[Cl:1][C:2]1[CH:8]=[CH:7][C:5]([NH2:6])=[CH:4][CH:3]=1.[CH:9]([CH2:11][O:12][C:13]1[CH:22]=[CH:21][C:16]([C:17]([O:19][CH3:20])=[O:18])=[CH:15][CH:14]=1)=O.C(B)#N.[Na]>CO>[Cl:1][C:2]1[CH:8]=[CH:7][C:5]([NH:6][CH2:9][CH2:11][O:12][C:13]2[CH:22]=[CH:21][C:16]([C:17]([O:19][CH3:20])=[O:18])=[CH:15][CH:14]=2)=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 78124-ChloroanilineHCID 11636984Methyl 4-formylmethyloxybenzoateHCID 101953985CID 101953985

生成物 1

HCID 15086593HCID 15086593、化合物収率 17.8%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

p-Chloroaniline (0.99 g) and methyl 4-formylmethoxybenzoate (1.5 g) were dissolved in anhydrous methanol (10 ml), and stirred at room temperature for 30 minutes. To the mixture was added sodium cyanoboron hydride (in solid form) (0.24 g) over a period of 30 minutes and further stirred for 30 minutes. After the reaction solution was concentrated under reduced pressure, water and chloroform were added thereto, and the mixture was separated into layers. The organic layer was concentrated under reduced pressure, and subjected to column chromatograpy on silica gel and eluted with chloroform to give the desired product (0.42 g).

後処理

  1. stirringfurther stirred for 30 minutes
  2. concentrationAfter the reaction solution was concentrated under reduced pressure, water and chloroform
  3. additionwere added
  4. customthe mixture was separated into layers
  5. concentrationThe organic layer was concentrated under reduced pressure
  6. washeluted with chloroform

出典と根拠

ORDレコード
ord-66f527c241c141639f84e1e49de3ab41
出典データセット
uspto-grants-1991_03
特許番号
US04999378

反応ノート

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