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Formic Acid → 1-carboxymethyl-3-hydroxy-2(1H)pyridinone

HRID 1871787
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HRID 1871787 반응식
C([O:3][C:4]([CH2:6][N:7]1[CH:12]=[CH:11][CH:10]=[C:9]([OH:13])[C:8]1=[O:14])=[O:5])C.C(O)=O>C(O)C.O>[C:4]([CH2:6][N:7]1[CH:12]=[CH:11][CH:10]=[C:9]([OH:13])[C:8]1=[O:14])([OH:5])=[O:3]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 284Formic AcidHCID 11127212ethyl 2-(3-hydroxy-2-oxopyridin-1(2H)-yl)acetate

생성물 1

HCID 100123081-carboxymethyl-3-hydroxy-2(1H)pyridinone수율 81.6%

시약·촉매·용매 1

HCID 19096565Water ethanol용매

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온도
60 °C

실험 절차

1-Ethoxycarbonylmethyl-3-hydroxypyrid-2-one (2 g) is dissolved in 15 ml of 1:2 v/v ethanol/water containing sufficient ammonium hydroxide to create a pH of 12.0. The solution is heated at 60° C. for 30 minutes, cooled, and acidified to pH 3.0 by the addition of formic acid. The solution is rotary evaporated to remove most of the ethanol and then freeze dried for 20 hours to remove the water, formic acid and ammonium formate. The resulting solid is recrystallised from water to yield white crystals (1.4 g), m.p. 203°-205° C.; νmax (nujol) 1540, 1590, 1640, 1695, 3240 cm-1 ; δ(d6DMSO) 4.5 (s, 2H), 5.95 (t, 1H), 6.6 (d, 1H), 7.0 (d, 1H).

후처리

  1. temperaturecooled
  2. customThe solution is rotary evaporated
  3. customto remove most of the ethanol
  4. customfreeze dried for 20 hours
  5. customto remove the water, formic acid and ammonium formate
  6. customThe resulting solid is recrystallised from water

출처 및 근거

ORD 기록
ord-002c8b98d40c4f0da5a4126074c24de0
출처 데이터셋
uspto-grants-2000_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
USRE036831

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