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4-Hydroxybenzaldehyde → HCID 77949816, 화합물

HRID 643196
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HRID 643196 반응식
[C:1]([CH2:3][C:4]([NH:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][C:12]([OH:14])=[O:13])=[O:5])#[N:2].[OH:15][C:16]1[CH:23]=[CH:22][C:19]([CH:20]=O)=[CH:18][CH:17]=1.N1CCCCC1>N1C=CC=CC=1>[OH:13][C:12](=[O:14])[CH2:11][CH2:10][CH2:9][CH2:8][CH2:7][NH:6][C:4](=[O:5])[C:3]([C:1]#[N:2])=[CH:20][C:19]1[CH:22]=[CH:23][C:16]([OH:15])=[CH:17][CH:18]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 1264-HydroxybenzaldehydeHCID 8082Piperidine2회HCID 85875172HCID 85875172, 화합물

생성물 1

HCID 77949816HCID 77949816, 화합물

시약·촉매·용매 1

HCID 1049Pyridine용매

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온도
50 °C

실험 절차

7.5 g (38 mmol 6-(cyanacetamido) hexanoic acid was dissolved in 50 ml pyridine. 4.6 g (38 mmol) 4-hydroxybenzaldehyde and 0.7 ml (7 mmol) piperidine were added to the solution and the reaction mixture was stirred for 2 hours at 50° C. A further aliquot of 0.4 ml piperidine was then added to the reaction and the solution was stirred at RT for 60 hours. The residue after evaporation of the pyridine was acidified with HCl (2N) and was extracted with ethyl acetate. The organic layer was poured into 300 ml of a saturated solution of sodium hydrogen carbonate. The aqueous layer was then carefully acidified with HCl (2N). The precipitated residue was filtered and washed with water. The dried product was crystallized from dioxane.

후처리

  1. stirringthe solution was stirred at RT for 60 hours
  2. customThe residue after evaporation of the pyridine
  3. extractionwas extracted with ethyl acetate
  4. additionThe organic layer was poured into 300 ml of a saturated solution of sodium hydrogen carbonate
  5. filtrationThe precipitated residue was filtered
  6. washwashed with water
  7. customThe dried product was crystallized from dioxane

출처 및 근거

ORD 기록
ord-c8138ec112ec4df4aadc4246127087e7
출처 데이터셋
uspto-grants-2010_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07700306B2

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