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

Tetrahydrofuran → [1-[2-[(3-Methyl-2-pyrazinyl)amino]ethyl]-4-piperidinyl]methyl 4-amino-5-chloro-2,3-dihydro-2,2-dimethyl-7-benzofurancarboxylate

HRID 392074
ノート
印刷プレビュー

反応式

HRID 392074 の反応式
[H-].[Na+].NC1C(Cl)=[CH:29][C:7]([C:8](OCC2CCN(CCCOC3C=CC(F)=CC=3)CC2)=O)=[C:6](OC)[CH:5]=1.[C:34]([N:41]1[CH:45]=[CH:44][N:43]=[CH:42]1)([N:36]1[CH:40]=[CH:39][N:38]=[CH:37]1)=O.[NH2:46][C:47]1[C:52]2[CH2:53][C:54]([CH3:57])([CH3:56])[O:55][C:51]=2[C:50]([C:58]([OH:60])=[O:59])=[CH:49][C:48]=1[Cl:61].[CH2:62]1COCC1>C(#N)C>[NH2:46][C:47]1[C:52]2[CH2:53][C:54]([CH3:57])([CH3:56])[O:55][C:51]=2[C:50]([C:58]([O:60][CH2:8][CH:7]2[CH2:29][CH2:42][N:43]([CH2:44][CH2:45][NH:41][C:34]3[C:37]([CH3:62])=[N:38][CH:39]=[CH:40][N:36]=3)[CH2:5][CH2:6]2)=[O:59])=[CH:49][C:48]=1[Cl:61]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 8028TetrahydrofuranHCID 24758Sodium hydrideHCID 682631,1'-CarbonyldiimidazoleHCID 106577584-Amino-5-chloro-2,2-dimethyl-2,3-dihydrobenzofuran-7-carboxylic acidHCID 22662758[1-[3-(4-Fluorophenoxy)propyl]-4-piperidinyl]methyl 4-amino-5-chloro-2-methoxybenzoate

生成物 1

HCID 11762499
[1-[2-[(3-Methyl-2-pyrazinyl)amino]ethyl]-4-piperidinyl]methyl 4-amino-5-chloro-2,3-dihydro-2,2-dimethyl-7-benzofurancarboxylate
収率 33%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

Sodium hydride (0.4 g) was added to a solution of intermediate 1 (2.3 g) in THF (65 ml). The mixture was stirred and refluxed for 3 hours, then cooled (solution I). 1,1′-Carbonylbis-1H-imidazole (1.65 g) was added to a solution of 4-amino-5-chloro-2,3-dihydro-2,2-dimethyl-7-benzofurancarboxylic acid (2.42 g) in ACN (65 ml), stirred at room temperature. This mixture was stirred for 2 hours at room temperature. The solvent was evaporated. The residue was dissolved in THF (65 ml) (solution II). At room temperature, solution (II) was poured out into solution (I) and the reaction mixture was stirred for 90 minutes at room temperature. The solvent was evaporated. The residue was partitioned between DCM and water. The organic layer was separated, dried, filtered and the solvent was evaporated. The residue was purified by column chromatography over silica gel (eluent: CH2Cl2/(CH3OH/NH3) 95/5). The pure fractions were collected and the solvent was evaporated. The residue was solidified in DIPE. The precipitate was filtered off and dried vacuum; 50° C.), yielding 1.58 g (33%) [1-[2-[(3-methyl-2-pyrazinyl)amino]ethyl]-4-piperidinyl]methyl 4-amino-5-chloro-2,3-dihydro-2,2-dimethyl-7-benzofurancarboxylate (compound 6).

後処理

  1. temperaturerefluxed for 3 hours
  2. stirringstirred at room temperature
  3. stirringThis mixture was stirred for 2 hours at room temperature
  4. customThe solvent was evaporated
  5. dissolutionThe residue was dissolved in THF (65 ml) (solution II)
  6. additionAt room temperature, solution (II) was poured out into solution (I)
  7. stirringthe reaction mixture was stirred for 90 minutes at room temperature
  8. customThe solvent was evaporated
  9. customThe residue was partitioned between DCM and water
  10. customThe organic layer was separated
  11. customdried
  12. filtrationfiltered
  13. customthe solvent was evaporated
  14. customThe residue was purified by column chromatography over silica gel (eluent: CH2Cl2/(CH3OH/NH3) 95/5)
  15. customThe pure fractions were collected
  16. customthe solvent was evaporated
  17. filtrationThe precipitate was filtered off
  18. customdried vacuum

出典と根拠

ORDレコード
ord-f7ef5d30f933440a96b5c6081fbd0b11
出典データセット
uspto-grants-2004_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06800628B2

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