4-Chloroaniline → HCID 15086593, 화합물

HRID 359081노트

반응식

HRID 359081 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 15086593HCID 15086593, 화합물수율 17.8%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-66f527c241c141639f84e1e49de3ab41
출처 데이터셋
uspto-grants-1991_03
특허 번호
US04999378

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