3,4-dihydro-2H-pyran → HCID 18648593, 화합물

HRID 467162노트

반응식

HRID 467162 반응식
[NH:1]1[C:5](=[O:6])[CH2:4][CH2:3][C@H:2]1[C:7]([N:9]1[CH2:15][CH2:14][CH2:13][C@H:10]1[CH2:11][OH:12])=[O:8].[O:16]1[CH:21]=[CH:20][CH2:19][CH2:18][CH2:17]1>C(#N)C.C1(C)C(S(O)(=O)=O)=CC=CC=1.N1C=CC=CC=1>[NH:1]1[C:5](=[O:6])[CH2:4][CH2:3][C@H:2]1[C:7]([N:9]1[CH2:15][CH2:14][CH2:13][C@H:10]1[CH2:11][O:12][CH:17]1[CH2:18][CH2:19][CH2:20][CH2:21][O:16]1)=[O:8]

참가 물질

5

반응물 2

HCID 80803,4-dihydro-2H-pyranHCID 18648590HCID 18648590, 화합물

생성물 1

HCID 18648593HCID 18648593, 화합물수율 110%

시약·촉매·용매 2

HCID 22058245HCID 22058245, 화합물촉매HCID 6342Acetonitrile용매

실험 절차

The thus obtained L-pyroglutamyl-L-prolinol (110 g, 0.519 mol) and dihydropyran (220 g, 2.62 mol) are dissolved in acetonitrile (2.75 l), and pyridine toluenesulfonate (11 g) is added under water-cooling. The mixture is stirred at room temperature for two days, and the reaction liquid is concentrated under reduced pressure, dissolved again in methylene chloride (1.5 l) and washed successively with 5% potassium carbonate (1 l) and water (1 l). The methylene chloride layer is dried over anhydrous magnesium sulfate and filtered. The filtrate is concentrated to dryness under reduced pressure to give N-pyroglutamyl-O-tetrahydropyranyl-L-prolinol (169 g, 110%).

후처리

  1. temperaturecooling
  2. customthe reaction liquid
  3. concentrationis concentrated under reduced pressure
  4. dissolutiondissolved again in methylene chloride (1.5 l)
  5. washwashed successively with 5% potassium carbonate (1 l) and water (1 l)
  6. dry with materialThe methylene chloride layer is dried over anhydrous magnesium sulfate
  7. filtrationfiltered
  8. concentrationThe filtrate is concentrated to dryness under reduced pressure

출처 및 근거

ORD 기록
ord-ec7759caaa49419185756baaae8d22e9
출처 데이터셋
uspto-grants-1992_10
특허 번호
US05158970

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