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Triethylamine → (E)-5,5-diphenyl-N-[4-(3-pyridinyl)butyl]-2,4-pentadienamide

HRID 2232777
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HRID 2232777 반응식
[C:1]1([C:7]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)=[C:8]=[C:9]=[CH:10][C:11]([OH:13])=O)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C(N(CC)CC)C.ClC(OCC)=O.[N:33]1[CH:38]=[CH:37][CH:36]=[C:35]([CH2:39][CH2:40][CH2:41][CH2:42][NH2:43])[CH:34]=1>O1CCCC1>[C:14]1([C:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)=[CH:8]/[CH:9]=[CH:10]/[C:11]([NH:43][CH2:42][CH2:41][CH2:40][CH2:39][C:35]2[CH:34]=[N:33][CH:38]=[CH:37][CH:36]=2)=[O:13])[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1
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참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 10928Ethyl chloroformateHCID 72927Pyridine, 3-(4-aminobutyl)-HCID 88605109HCID 88605109, 화합물

생성물 1

HCID 14347363(E)-5,5-diphenyl-N-[4-(3-pyridinyl)butyl]-2,4-pentadienamide수율 38.4%

시약·촉매·용매 1

HCID 8028
Tetrahydrofuran
용매
3회

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온도
0 °C

실험 절차

To a stirred solution of 5,5-diphenyl-2,4-pentadienenoic acid (6.00 g) and triethylamine (3.7 mL) in dry tetrahydrofurane (40 mL) at 0°- C. was added a solution of ethyl chloroformate (2.37 mL) in tetrahydrofurane (15 mL) dropwise such that the reaction temperature was maintained at 0° C. After the addition was complete, the reaction was stirred at 0° C. for 15 minutes, then a solution of 3-pyridinebutanamine (3.78 g) in tetrahydrofurane (20 mL) was added dropwise while keeping the reaction at 0° C. The mixture was stirred at 0° C. for 1 hour and then at room temperature for 2 hours before the precipitated triethylamine hydrochloride was removed by filtration. The evaporated filtrate was partitioned between 1N hydrochloric acid solution (80 mL) and ether (80 mL). After the ethereal extract was discarded, the aqueous layer was basified with 4N sodium hydroxide (30 mL) and extracted with ether (4×100 mL). Evaporation of the dried (K2CO3) organic extracts afforded the crude amide which was purified by HPLC (hexane-ethyl acetate-triethylamine; 25:75:2) to provide 3.55 g of (E)-5,5-diphenyl-N-[4-(3-pyridinyl)butyl]-2,4-pentadienamide 0.2 molar hydrate as an oil.

후처리

  1. customat 0°
  2. additionAfter the addition
  3. customthe reaction at 0° C
  4. stirringThe mixture was stirred at 0° C. for 1 hour
  5. customat room temperature for 2 hours before the precipitated triethylamine hydrochloride was removed by filtration
  6. customThe evaporated filtrate was partitioned between 1N hydrochloric acid solution (80 mL) and ether (80 mL)
  7. extractionAfter the ethereal extract
  8. extractionextracted with ether (4×100 mL)
  9. customEvaporation of the
  10. dry with materialdried (K2CO3) organic extracts
  11. customafforded the crude amide which
  12. customwas purified by HPLC (hexane-ethyl acetate-triethylamine; 25:75:2)

출처 및 근거

ORD 기록
ord-68e5930642be4b32bf8954d13ed32ebc
출처 데이터셋
uspto-grants-1988_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04788206

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