Water → {4-[2-(Pyrrolidin-1-yl)ethyl]-1H-pyrrol-2-yl}methanol

HRID 1093983노트

반응식

HRID 1093983 반응식
[N:1]1([CH2:6][CH2:7][C:8]2[CH:9]=[C:10]([C:13](OCC)=[O:14])[NH:11][CH:12]=2)[CH2:5][CH2:4][CH2:3][CH2:2]1.[H-].[Al+3].[Li+].[H-].[H-].[H-].[OH-].[Na+].O>C1COCC1>[N:1]1([CH2:6][CH2:7][C:8]2[CH:9]=[C:10]([CH2:13][OH:14])[NH:11][CH:12]=2)[CH2:5][CH2:4][CH2:3][CH2:2]1

참가 물질

6

반응물 4

HCID 962WaterHCID 14798Sodium HydroxideHCID 21226445Aluminium lithium hydrideHCID 66636407Ethyl 4-[2-(pyrrolidin-1-yl)ethyl]-1H-pyrrole-2-carboxylate

생성물 1

HCID 66636497{4-[2-(Pyrrolidin-1-yl)ethyl]-1H-pyrrol-2-yl}methanol

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of the product obtained in Step H (0.2 g) in THF (10 ml) at 0° C. there is added, in portions, lithium aluminium hydride. After stirring for 3 hours at ambient temperature, the reaction mixture is hydrolysed at 0° C. with aq. NaOH solution and water. After filtration, the filtrate is evaporated to dryness and the residue obtained is purified on silica gel (SiO2: gradient CH2Cl2/MeOH with the addition of 1.4N NH3 in the MeOH) to yield the title product, which is used directly in the next Step.

후처리

  1. filtrationAfter filtration
  2. customthe filtrate is evaporated to dryness
  3. customthe residue obtained
  4. customis purified on silica gel (SiO2
  5. additiongradient CH2Cl2/MeOH with the addition of 1.4N NH3 in the MeOH)

출처 및 근거

ORD 기록
ord-aa16bb0e76574c2b91610ac24b24cf1d
출처 데이터셋
uspto-grants-2012_03
특허 번호
US08133889B2

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