Ethanol → 2-Hydroxymethyl-5-methylpyrazine-4-oxide

HRID 2286699

반응식

HRID 2286699 반응식
[C:1]([C:4]1[CH:9]=[N+:8]([O-:10])[C:7]([CH3:11])=[CH:6][N:5]=1)(O)=[O:2].B#B.C(O)C.C([O-])([O-])=O.[K+].[K+]>COCCOCCOC.O1CCCC1>[OH:2][CH2:1][C:4]1[CH:9]=[N+:8]([O-:10])[C:7]([CH3:11])=[CH:6][N:5]=1

참가 물질

7

반응물 4

HCID 702EthanolHCID 11430Potassium CarbonateHCID 5310993AcipimoxHCID 6328200Diboron

생성물 1

HCID 130230052-Hydroxymethyl-5-methylpyrazine-4-oxide수율 88%

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매HCID 8150Diglyme용매

반응 조건

온도
0 °C

실험 절차

Method B--To a solution of 2-carboxy-5-methyl-pyrazine-4-oxide (1.5 g) in diethylene glycol dimethyl ether (80 ml) addition was made at 0° C. under an atmosphere of nitrogen of a solution (1 M) of diborane in tetrahydrofuran (30 ml). To the reaction mixture maintained for 3 hours at 0° C. and 1 hour at room temperature, cautious addition was made of ethanol (50 ml) and then of a 0.5 M solution of alcoholic potash (25 ml). The resultant solution after evaporation at reduced pressure was taken up with chloroform which, on evaporation to dryness, gave 1.2 g of 2-hydroxymethyl-5-methyl-pyrazine-4-oxide.

후처리

  1. additioncautious addition
  2. customThe resultant solution after evaporation at reduced pressure
  3. customwas taken up with chloroform which, on evaporation to dryness

출처 및 근거

ORD 기록
ord-97dcf43bbb0f44b29e1906d04cb7bd67
출처 데이터셋
uspto-grants-1981_05
특허 번호
US04267327

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