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

HRID 1577503

반응식

HRID 1577503 반응식
[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]

참가 물질

7

반응물 4

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

생성물 1

HCID 205709095-(Dimethylaminomethyl)-4-methyl-2-furanmethanol수율 63.9%

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매2회HCID 8058Hexane용매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-52f9c2e5704e4df9816d527246f83d59
출처 데이터셋
uspto-grants-1981_09
특허 번호
US04288443

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