Acetonitrile → HCID 67045661, 화합물

HRID 1943102노트

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HRID 1943102 반응식
Cl[CH2:2][CH2:3][CH2:4][O:5][C:6]1[CH:19]=[CH:18][C:9]([C:10]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)=[O:11])=[CH:8][CH:7]=1.[CH2:20](N)[CH2:21][CH2:22][CH2:23][CH2:24][CH3:25].C(#[N:29])C>>[CH3:20][CH2:21][CH:22]([NH:29][CH2:2][CH2:3][CH2:4][O:5][C:6]1[CH:19]=[CH:18][C:9]([C:10]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)=[O:11])=[CH:8][CH:7]=1)[CH2:23][CH2:24][CH3:25]

참가 물질

4

반응물 3

HCID 6342AcetonitrileHCID 8102HexylamineHCID 10934655HCID 10934655, 화합물

생성물 1

HCID 67045661HCID 67045661, 화합물

반응 조건

온도
70 °C

실험 절차

10 g (36 mmol) 4-(3-chloropropoxy)benzophenone was dissolved in 100 mL acetonitrile. 36.4 g (0.36 mol) n.-hexyl amine was added and the mixture was heated to 70° C. for 20 hours. The solvent was evaporated under reduced pressure. The oily residue was treated with 500 mL water. The mixture was acidified to pH=1 and stirred for 16 hours at room temperature. The precipitated compounds were isolated by filtration and washed with 200 mL 1 N HCl. The precipitate was treated with 200 mL 1 N NaOH. The mixture was extracted with 200 mL methylene chloride. The organic fraction was dried over MgSO4 and the solvent was evaporated under reduced pressure. The crude 4-[(3-hexylamino)propoxy]benzophenone was purified by preparative column chromatography on a Prochrom LC80 column, using Kromasil Si 60A 10 mm as silica and a gradient elution from methylene chloride to methylene chloride/methanol 68/32 at a flow rate of 150 mL per minute. 3.9 g of 4-[(3-hexylamino)propoxy]benzophenone was isolated.

후처리

  1. customThe solvent was evaporated under reduced pressure
  2. additionThe oily residue was treated with 500 mL water
  3. customThe precipitated compounds were isolated by filtration
  4. washwashed with 200 mL 1 N HCl
  5. additionThe precipitate was treated with 200 mL 1 N NaOH
  6. extractionThe mixture was extracted with 200 mL methylene chloride
  7. dry with materialThe organic fraction was dried over MgSO4
  8. customthe solvent was evaporated under reduced pressure
  9. customThe crude 4-[(3-hexylamino)propoxy]benzophenone was purified by preparative column chromatography on a Prochrom LC80 column
  10. washa gradient elution from methylene chloride to methylene chloride/methanol 68/32 at a flow rate of 150 mL per minute

출처 및 근거

ORD 기록
ord-7833d31d31eb4ee49387c89c594402e6
출처 데이터셋
uspto-grants-2013_03
특허 번호
US08389769B2

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