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3-(Piperazin-1-yl)propane-1,2-diol → 4-[4-(2,3-Dihydroxypropyl)piperazin-1-yl]pyrimidine-5-carboxylic acid ethyl ester dihydrochloride

HRID 231772
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HRID 231772 반응식
[OH:1][CH:2]([CH2:10][OH:11])[CH2:3][N:4]1[CH2:9][CH2:8][NH:7][CH2:6][CH2:5]1.[CH2:12]([O:14][C:15]([C:17]1[C:18]([Cl:23])=[N:19][CH:20]=[N:21][CH:22]=1)=[O:16])[CH3:13]>O1CCOCC1>[ClH:23].[ClH:23].[CH2:12]([O:14][C:15]([C:17]1[C:18]([N:7]2[CH2:8][CH2:9][N:4]([CH2:3][CH:2]([OH:1])[CH2:10][OH:11])[CH2:5][CH2:6]2)=[N:19][CH:20]=[N:21][CH:22]=1)=[O:16])[CH3:13]
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참가 물질

4

반응물 2

HCID 1110023-(Piperazin-1-yl)propane-1,2-diolHCID 12684326Ethyl 4-chloropyrimidine-5-carboxylate

생성물 1

HCID 678614724-[4-(2,3-Dihydroxypropyl)piperazin-1-yl]pyrimidine-5-carboxylic acid ethyl ester dihydrochloride

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

Grams 7.4 of 1-(2,3-dihydroxypropyl)piperazine and 4.3 g of 4-chloropyrimidine-5-carboxylic acid ethyl ester were warmed to 90° C. for 45 minutes in 100 ml dioxane. The reaction mixture was then settled, the supernatant liquor evaporated to dryness and the residue dissolved in hydrochloric ethanol and diluted with isopropanol until complete precipitation. By addition of 95° ethanol, the so formed gum crystallized and 4 g of 4-[4-(2,3-dihydroxypropyl)piperazin-1-yl]pyrimidine-5-carboxylic acid ethyl ester dihydrochloride, melting at 190°-193° C. (with decomposition), were obtained.

후처리

  1. customthe supernatant liquor evaporated to dryness
  2. dissolutionthe residue dissolved in hydrochloric ethanol
  3. additiondiluted with isopropanol until complete precipitation
  4. additionBy addition of 95° ethanol
  5. customthe so formed gum crystallized

출처 및 근거

ORD 기록
ord-456c26e5656e48b5be33bab1ac5493e5
출처 데이터셋
uspto-grants-1989_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04849422

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