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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
ノート
印刷プレビュー

反応式

HRID 231772 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-456c26e5656e48b5be33bab1ac5493e5
出典データセット
uspto-grants-1989_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04849422

反応ノート

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