2-Nitrothiophene-4-carboxaldehyde → HCID 9860933, 화합물

HRID 1604735노트

반응식

HRID 1604735 반응식
[N+:1]([C:4]1[S:5][CH:6]=[C:7]([CH:9]=[O:10])[CH:8]=1)([O-:3])=[O:2].[P:11]([O-:18])([O:15][CH2:16][CH3:17])[O:12][CH2:13][CH3:14]>CO>[N+:1]([C:4]1[S:5][CH:6]=[C:7]([CH:9]([P:11](=[O:18])([O:15][CH2:16][CH3:17])[O:12][CH2:13][CH3:14])[OH:10])[CH:8]=1)([O-:3])=[O:2]

참가 물질

4

반응물 2

HCID 1447302-Nitrothiophene-4-carboxaldehydeHCID 3780918Diethylphosphite

생성물 1

HCID 9860933HCID 9860933, 화합물수율 72.4%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A solution containing 2-nitro-4-thiophenecarboxaldehyde (2.61 g, 16.6 mmol), diethyl phosphite (2.14 mL, 16.6 mmol), and methanol (5 mis) was adsorbed onto excess basic alumina. After 16 hours the product was extracted with methylene chloride, concentrated and purified by column chromatography (silica gel). Elution with methylene chloride-methanol 19:1 gave the product (3.55 g) as an oil. 1H NMR (CDC13): d, 5.05 (dd,1H,PCH), 4.15 (m,4H,CH2), 1.33 (dt,6H,CH3). MS (DCl): 296 (MH+). C9H14NO6PS.

후처리

  1. extractionAfter 16 hours the product was extracted with methylene chloride
  2. concentrationconcentrated
  3. custompurified by column chromatography (silica gel)
  4. washElution with methylene chloride-methanol 19:1

출처 및 근거

ORD 기록
ord-779957d2d513477bbaccf3c0fa5ea775
출처 데이터셋
uspto-grants-1999_11
특허 번호
US05994563

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