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Glycolic Acid → (3H-imidazo(4,5-b)pyridin-2-yl)methanol

HRID 2083986
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HRID 2083986 반응식
[NH2:1][C:2]1[C:7]([NH2:8])=[CH:6][CH:5]=[CH:4][N:3]=1.[C:9](O)(=O)[CH2:10][OH:11].O>C1(C)C=C(C)C=C(C)C=1>[OH:11][CH2:10][C:9]1[NH:8][C:7]2[CH:6]=[CH:5][CH:4]=[N:3][C:2]=2[N:1]=1
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참가 물질

5

반응물 3

HCID 757Glycolic AcidHCID 962WaterHCID 99562,3-Diaminopyridine

생성물 1

HCID 1282496(3H-imidazo(4,5-b)pyridin-2-yl)methanol

시약·촉매·용매 1

HCID 7947Mesitylene용매

실험 절차

using a Dan-Stark separator, 2,3-diaminopyridine (54.6 g; 0.5 mol) and glycolic acid (38 g; 0.5 mol) in 700 ml of mesitylene were boiled under reflux until the calculated amount of water had separated off. The mixture was then cooled to room temperature, and the resulting precipitate was filtered off with suction and, with addition of activated carbon, boiled in 800 ml of water for 15 min. The hot suspension was filtered and once more cooled to room temperature, and the colourless crystals that precipitated out were filtered off with suction and dried. Yield: 56.4 g (75%).

후처리

  1. customhad separated off
  2. filtrationthe resulting precipitate was filtered off with suction and, with addition of activated carbon
  3. filtrationThe hot suspension was filtered
  4. temperatureonce more cooled to room temperature
  5. customthe colourless crystals that precipitated out
  6. filtrationwere filtered off with suction
  7. customdried

출처 및 근거

ORD 기록
ord-ccbd2eccc5e24b8bb077e0f6077b6835
출처 데이터셋
uspto-grants-2004_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06716849B1

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