ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Hydrochloric Acid → 1,3,4,5-tetrahydro-1-{1-[(4-methyl-4H,6H-pyrrolo[1,2-a][4,1]benzoxazepin-4-yl)-methyl]-4-piperidinyl}-2H-imidazol-2-one

HRID 845382
ノート
印刷プレビュー

反応式

HRID 845382 の反応式
[CH:1]([C:3]1([CH3:17])[O:9][CH2:8][C:7]2[CH:10]=[CH:11][CH:12]=[CH:13][C:6]=2[N:5]2[CH:14]=[CH:15][CH:16]=[C:4]12)=O.Cl.[NH:19]1[CH2:24][CH2:23][CH:22]([N:25]2[CH2:29][CH2:28][NH:27][C:26]2=[O:30])[CH2:21][CH2:20]1.C([BH3-])#N.[Na+]>CO>[CH3:17][C:3]1([CH2:1][N:19]2[CH2:20][CH2:21][CH:22]([N:25]3[CH2:29][CH2:28][NH:27][C:26]3=[O:30])[CH2:23][CH2:24]2)[O:9][CH2:8][C:7]2[CH:10]=[CH:11][CH:12]=[CH:13][C:6]=2[N:5]2[CH:14]=[CH:15][CH:16]=[C:4]12
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 313Hydrochloric Acid2 回HCID 5003444Sodium cyanoborohydrideHCID 130317571-(Piperidin-4-yl)imidazolidin-2-oneHCID 141830784-formyl-4-methyl-4H,6H-pyrrolo[1,2-a][4,1]benzoxazepine

生成物 1

HCID 141830791,3,4,5-tetrahydro-1-{1-[(4-methyl-4H,6H-pyrrolo[1,2-a][4,1]benzoxazepin-4-yl)-methyl]-4-piperidinyl}-2H-imidazol-2-one

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of 4.5 g of 4-formyl-4-methyl-4H,6H-pyrrolo[1,2-a][4,1]benzoxazepine in 50 ml of methanol is added 3.6 ml of 5.5N methanolic HCl and 3.4 g of 1,3,4,5-tetrahydro-1-(4-piperidinyl)-2H-imidazol-2-one followed by 900 mg of sodium cyanoborohydride. The reaction mixture is allowed to stir at room temperature for 8 days. 2 ml of conc. HCl is added to the reaction mixture and the solvent is removed by evaporation under reduced pressure. The residue is dissolved in 150 ml water and washed with 150 ml of 1:1 ethyl acetate-ether mixture. The aqueous phase is separated, basified with dilute sodium hydroxide to pH 9 and extracted with 2×150 ml of ethyl acetate. The combined ethyl acetate extracts are dried over anhydrous MgSO4, filtered, and the solvent is removed by evaporation under reduced pressure to yield 1,3,4,5-tetrahydro-1-{1-[(4-methyl-4H,6H-pyrrolo[ 1,2-a][4,1]benzoxazepin-4-yl)-methyl]-4-piperidinyl}-2H-imidazol-2-one which is characterized as its maleate salt, m.p. 197°-199°.

後処理

  1. customthe solvent is removed by evaporation under reduced pressure
  2. dissolutionThe residue is dissolved in 150 ml water
  3. washwashed with 150 ml of 1:1 ethyl acetate-ether mixture
  4. customThe aqueous phase is separated
  5. extractionextracted with 2×150 ml of ethyl acetate
  6. dry with materialThe combined ethyl acetate extracts are dried over anhydrous MgSO4
  7. filtrationfiltered
  8. customthe solvent is removed by evaporation under reduced pressure

出典と根拠

ORDレコード
ord-75414067f18d4915a0a190e7ac66f456
出典データセット
uspto-grants-1988_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04758559

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート