Sodium Hydroxide → 4-[(1-Methylpyrrolidin-2-yl)methyl]aniline

HRID 1278083ノート

反応式

HRID 1278083 の反応式
[NH2:1][C:2]1[CH:15]=[CH:14][C:5]([CH2:6][CH:7]2[N:11]([CH3:12])[C:10](=O)[CH2:9][CH2:8]2)=[CH:4][CH:3]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-].[OH-].[Na+]>O1CCCC1>[NH2:1][C:2]1[CH:15]=[CH:14][C:5]([CH2:6][CH:7]2[CH2:8][CH2:9][CH2:10][N:11]2[CH3:12])=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 21226445Aluminium lithium hydrideHCID 234525985-(4-Aminobenzyl)-1-methylpyrrolidin-2-one

生成物 1

HCID 131869044-[(1-Methylpyrrolidin-2-yl)methyl]aniline

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Boil 2.04 g of 5-(4-aminobenzyl)-1-methylpyrrolidin-2-one and 0.7 g of lithium aluminum hydride under reflux for 20 hours in 20 ml of tetrahydrofuran. Decompose the resulting reaction product by admixing it with ice water. After adding 10 ml of 6 N sodium hydroxide solution to the decomposed product, extract it with diethyl ether. Dry the ether extract over sodium sulfate and concentrate it to obtain the title compound in free-base form. Convert the thus-obtained base into the dihydrochloride [m.p. (from methanol/ether)>242° (decomp.)] with methanol/ethereal hydrochloric acid.

後処理

  1. customthe resulting reaction product
  2. extractionextract it with diethyl ether
  3. dry with materialDry the ether
  4. extractionextract over sodium sulfate
  5. concentrationconcentrate it

出典と根拠

ORDレコード
ord-9ce85bc1244541b58f3a82f1a9a0411a
出典データセット
uspto-grants-1981_07
特許番号
US04279918

反応ノート

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