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

HRID 241718노트

반응식

HRID 241718 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 stiffing 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-86a6de7333f446cd918bf225157b2e3a
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08653073B2

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