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HCID 13105519、化合物 → 1-(2-(Piperazin-1-YL)ethyl)-1,3-dihydro-2H-benzo[D]imidazol-2-one

HRID 2050283
ノート
印刷プレビュー

反応式

HRID 2050283 の反応式
C1(C[N:8]2[CH2:13][CH2:12][N:11]([CH2:14][CH2:15][N:16]3[C:20]4[CH:21]=[CH:22][CH:23]=[CH:24][C:19]=4[NH:18][C:17]3=[O:25])[CH2:10][CH2:9]2)C=CC=CC=1.[H][H]>[Pd].CO>[N:11]1([CH2:14][CH2:15][N:16]2[C:20]3[CH:21]=[CH:22][CH:23]=[CH:24][C:19]=3[NH:18][C:17]2=[O:25])[CH2:12][CH2:13][NH:8][CH2:9][CH2:10]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 13105519HCID 13105519、化合物HCID 178418361HCID 178418361、化合物

生成物 1

HCID 131056241-(2-(Piperazin-1-YL)ethyl)-1,3-dihydro-2H-benzo[D]imidazol-2-one

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

A mixture of 79 parts of 1,3-dihydro-1-{2-[4-(phenylmethyl)-1-piperazinyl]ethyl}-2H-benzimidazol-2-one and 320 parts of methanol is hydrogenated at normal pressure and at room temperature with 10 parts of palladium-on-charcoal catalyst 10%. After the calculated amount of hydrogen is taken up, the catalyst is filtered off and the filtrate is evaporated. The oily residue is alkalized with ammonium hydroxide and a small amount of water is added. The product is extracted with trichloromethane. The extract is dried, filtered and evaporated. The oily residue solidifies on triturating in 4-methyl-2-pentanone. The product is filtered off and dried, yielding 1,3-dihydro-1-[2-(1-piperazinyl)ethyl]-2H-benzimidazol-2-one; mp. 122.6° C.

後処理

  1. filtrationthe catalyst is filtered off
  2. customthe filtrate is evaporated
  3. additiona small amount of water is added
  4. extractionThe product is extracted with trichloromethane
  5. customThe extract is dried
  6. filtrationfiltered
  7. customevaporated
  8. customon triturating in 4-methyl-2-pentanone
  9. filtrationThe product is filtered off
  10. customdried

出典と根拠

ORDレコード
ord-ad876ebba9234333903bb10ca72cb7c3
出典データセット
uspto-grants-1980_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04200641

反応ノート

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