(+/-)-5-(2,5-Dioxo-4-imidazolidinylmethyl)-3-(1-methyl-4-piperidyl)-1H-indole → (+/-)-3-[3-(1-Methyl-4-piperidyl)-1H-indol-5-yl]alanine

HRID 128968

反応式

HRID 128968 の反応式
O=C1[NH:6][CH:5]([CH2:7][C:8]2[CH:9]=[C:10]3[C:14](=[CH:15][CH:16]=2)[NH:13][CH:12]=[C:11]3[CH:17]2[CH2:22][CH2:21][N:20]([CH3:23])[CH2:19][CH2:18]2)[C:4](=[O:24])N1.[OH2:25].[OH-].[Ba+2].[OH-]>O>[CH3:23][N:20]1[CH2:21][CH2:22][CH:17]([C:11]2[C:10]3[C:14](=[CH:15][CH:16]=[C:8]([CH2:7][C@@H:5]([C:4]([OH:24])=[O:25])[NH2:6])[CH:9]=3)[NH:13][CH:12]=2)[CH2:18][CH2:19]1

参加物

4

反応物 2

HCID 15233277(+/-)-5-(2,5-Dioxo-4-imidazolidinylmethyl)-3-(1-methyl-4-piperidyl)-1H-indoleHCID 17749100Barium hydroxide, monohydrate

生成物 1

HCID 22852202(+/-)-3-[3-(1-Methyl-4-piperidyl)-1H-indol-5-yl]alanine収率 58.7%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A solution of the product from step (d) (2.4 g) and barium hydroxide hydrate (8.4 g) in water (50 ml) was refluxed for 72 hours, then cooled and evaporated in vacuo. The residue was taken up in hot methanol and filtered to remove barium salts. The filtrate was evaporated in vacuo, the residue dissolved in water and dry ice added to precipitate barium carbonate. The latter was filtered off and the filtrate evaporated in vacuo to give the desired product as a yellow foam (1.3 g).

後処理

  1. temperaturecooled
  2. customevaporated in vacuo
  3. filtrationfiltered
  4. customto remove barium salts
  5. customThe filtrate was evaporated in vacuo
  6. dissolutionthe residue dissolved in water
  7. additiondry ice added
  8. customto precipitate barium carbonate
  9. filtrationThe latter was filtered off
  10. customthe filtrate evaporated in vacuo

出典と根拠

ORDレコード
ord-1ed5480966f7465eb26b1e10832e79ae
出典データセット
uspto-grants-1995_11
特許番号
US05466699

関連ノート

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