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Dipropylamine → (S)-2-(4-Chlorophenyl)-alpha-methyl-N,N-dipropyl-3H-imidazo[4,5-b]pyridine-3-acetamide

HRID 2351732
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HRID 2351732 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:16]([CH:17]([CH3:21])[C:18]([OH:20])=O)[C:11]3=[N:12][CH:13]=[CH:14][CH:15]=[C:10]3[N:9]=2)=[CH:4][CH:3]=1.C(N1C=CN=C1)(N1C=CN=C1)=O.[CH2:34]([NH:37][CH2:38][CH2:39][CH3:40])[CH2:35][CH3:36]>O1CCCC1>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[N:16]([C@@H:17]([CH3:21])[C:18]([N:37]([CH2:38][CH2:39][CH3:40])[CH2:34][CH2:35][CH3:36])=[O:20])[C:11]3=[N:12][CH:13]=[CH:14][CH:15]=[C:10]3[N:9]=2)=[CH:6][CH:7]=1
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참가 물질

5

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HCID 8902DipropylamineHCID 682631,1'-CarbonyldiimidazoleHCID 143904264-chlorophenyl-alpha-methyl-3H-imidazo[4,5-b]pyridine-3-acetic acid

생성물 1

HCID 14390410(S)-2-(4-Chlorophenyl)-alpha-methyl-N,N-dipropyl-3H-imidazo[4,5-b]pyridine-3-acetamide수율 52.1%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

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온도
50 °C

실험 절차

A solution of (S)-2-(4-chlorophenyl-α-methyl-3H-imidazo[4,5-b]pyridine-3-acetic acid (5.0 g, 0.0166 mole), 1,1'-carbonyldiimidazole (3.21 g, 0.0198 mole) and dry tetrahydrofuran (100 ml) was stirred at room temperature for 3 hours with nitrogen bubbling through it. A solution of dipropylamine (5.04 g, 0.050 mole) in tetrahydrofuran (7 ml) was added and the solution was heated at 50° C. overnight under nitrogen. The solvents were evaporated under reduced pressure and the resulting oil was partitioned between ethyl acetate (50 ml) and water (50 ml). The layers were separated and the aqueous layer was re-extracted with ethyl acetate (50 ml). The combined organic layers were washed once with water (50 ml) followed by two (50 ml) portions of 5% potassium hydroxide solution and then by water again (50 ml). The organic layer was dried over magnesium sulfate, charcoaled, filtered and evaporated to an oil which was crystallized from hot isopropyl ether. The solid was collected by filtration, and dried under high vacuum at room temperature to give 3.33 g (52%) of title compound, mp 96°-99° C.

후처리

  1. customThe solvents were evaporated under reduced pressure
  2. customthe resulting oil was partitioned between ethyl acetate (50 ml) and water (50 ml)
  3. customThe layers were separated
  4. extractionthe aqueous layer was re-extracted with ethyl acetate (50 ml)
  5. washThe combined organic layers were washed once with water (50 ml)
  6. dry with materialThe organic layer was dried over magnesium sulfate
  7. filtrationfiltered
  8. customevaporated to an oil which
  9. customwas crystallized from hot isopropyl ether
  10. filtrationThe solid was collected by filtration
  11. customdried under high vacuum at room temperature

출처 및 근거

ORD 기록
ord-75974183da0a449ba55a1010605f8630
출처 데이터셋
uspto-grants-1989_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04873251

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