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

HRID 1093983ノート

反応式

HRID 1093983 の反応式
[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

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-aa16bb0e76574c2b91610ac24b24cf1d
出典データセット
uspto-grants-2012_03
特許番号
US08133889B2

反応ノート

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