Formaldehyde → 5-(Dimethylaminomethyl)-4-methyl-2-furanmethanol

HRID 1577503

反応式

HRID 1577503 の反応式
[CH3:1][N:2]([CH3:10])[CH2:3][C:4]1[O:5][CH:6]=[CH:7][C:8]=1[CH3:9].C([Li])CCC.[CH2:16]=[O:17].O>O1CCCC1.CCCCCC>[CH3:1][N:2]([CH2:3][C:4]1[O:5][C:6]([CH2:16][OH:17])=[CH:7][C:8]=1[CH3:9])[CH3:10]

参加物

7

反応物 4

HCID 712FormaldehydeHCID 962WaterHCID 100347492-Dimethylaminomethyl-3-methylfuranHCID 178418339Butyllithium

生成物 1

HCID 205709095-(Dimethylaminomethyl)-4-methyl-2-furanmethanol収率 63.9%

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒2 回HCID 8058Hexane溶媒

実験手順

A solution of N,N,3-trimethyl-2-furanmethanamine (10.3 g) in dry tetrahydrofuran (200 ml) under nitrogen was treated over 2 hr with 1.6 M n-butyl lithium in hexane 846.2 ml) at -40° to -45° C. After stirring for 2 hr at room temperature paraformaldehyde (2.3 g) in dry tetrahydrofuran (100 ml) was added and the solution stirred overnight. Water (10 ml) was added and the solvent evaporated. Ethyl acetate (200 ml) and sodium sulphate were added and the organic phase was evaporated giving an oily residue which was distilled (85°/0.1 mm) affording the title compound (8 g).

後処理

  1. additionwas added
  2. customthe solvent evaporated
  3. additionEthyl acetate (200 ml) and sodium sulphate were added
  4. customthe organic phase was evaporated
  5. customgiving an oily residue which
  6. distillationwas distilled (85°/0.1 mm)

出典と根拠

ORDレコード
ord-52f9c2e5704e4df9816d527246f83d59
出典データセット
uspto-grants-1981_09
特許番号
US04288443

関連ノート

読み込み中…