Potassium Hydroxide → HCID 14856031、化合物

HRID 1032696ノート

反応式

HRID 1032696 の反応式
[OH-:1].[K+].[CH2:3]([N:10]1[CH2:15][CH2:14][N:13]([C:16]2[N:21]=[C:20]([CH2:22]Cl)[C:19]([C:24]([O:26]CC)=[O:25])=[CH:18][N:17]=2)[CH2:12][CH2:11]1)[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1>C(O)C>[CH2:3]([N:10]1[CH2:15][CH2:14][N:13]([C:16]2[N:21]=[C:20]([CH2:22][OH:1])[C:19]([C:24]([OH:26])=[O:25])=[CH:18][N:17]=2)[CH2:12][CH2:11]1)[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1

参加物

4

反応物 2

HCID 14797Potassium HydroxideHCID 13769878Ethyl 4-(chloromethyl)-2-[4-(phenylmethyl)-1-piperazinyl]-5-pyrimidinecarboxylate

生成物 1

HCID 14856031HCID 14856031、化合物収率 44.2%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Ethanol (80 ml) and 2.64 g (40.0 mmoles) of 85% potassium hydroxide were added to 5.0 g (13.3 mmoles) of ethyl 2-(4-benzylpiperazino)-4-chloromethylpyrimidine-5-carboxylate (produced in accordance with Referential Example 41 of Japanese Laid-Open Patent Publication No. 140568/1986), and the mixture was refluxed for 30 minutes. Ethanol was evaporated under reduced pressure. The residue was dissolved in water, and adjusted to pH about 4 with concentrated hydrochloric acid. The crystals that formed were collected by filtration, and washed with acetone to give 1.93 g (yield 44%) of 2-(4-benzylpiperazino)-4-hydroxymethylpyrimidine-5-carboxylic acid as crystals.

後処理

  1. customproduced in accordance with Referential Example 41 of Japanese Laid-Open Patent Publication No
  2. temperature140568/1986), and the mixture was refluxed for 30 minutes
  3. customEthanol was evaporated under reduced pressure
  4. dissolutionThe residue was dissolved in water
  5. customThe crystals that formed
  6. filtrationwere collected by filtration
  7. washwashed with acetone

出典と根拠

ORDレコード
ord-f93eced4a9424a3bbdb3a0f25d70b4d8
出典データセット
uspto-grants-1990_09
特許番号
US04959368

反応ノート

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