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

Sodium Hydroxide → tert-butyl (2S)-2-[(4-{[(3,4-dichlorophenyl)amino]-carbonyl}piperazin-1-yl)methyl]morpholine-4-carboxylate

HRID 2371158
ノート
印刷プレビュー

反応式

HRID 2371158 の反応式
CC(OI1(OC(C)=O)(OC(C)=O)OC(=O)C2C=CC=CC1=2)=O.O[CH2:24][C@@H:25]1[O:30][CH2:29][CH2:28][N:27]([C:31]([O:33][C:34]([CH3:37])([CH3:36])[CH3:35])=[O:32])[CH2:26]1.S([O-])([O-])(=O)=S.[Na+].[Na+].Cl.[Cl:46][C:47]1[CH:48]=[C:49]([NH:54][C:55]([N:57]2[CH2:62][CH2:61][NH:60][CH2:59][CH2:58]2)=[O:56])[CH:50]=[CH:51][C:52]=1[Cl:53].C(N(CC)C(C)C)(C)C.[BH-](OC(C)=O)(OC(C)=O)OC(C)=O.[Na+].[OH-].[Na+]>C(Cl)Cl>[Cl:46][C:47]1[CH:48]=[C:49]([NH:54][C:55]([N:57]2[CH2:62][CH2:61][N:60]([CH2:24][C@@H:25]3[O:30][CH2:29][CH2:28][N:27]([C:31]([O:33][C:34]([CH3:35])([CH3:36])[CH3:37])=[O:32])[CH2:26]3)[CH2:59][CH2:58]2)=[O:56])[CH:50]=[CH:51][C:52]=1[Cl:53]
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 7

HCID 14798Sodium HydroxideHCID 24477Sodium ThiosulfateHCID 81531DiisopropylethylamineHCID 159087TriacetoxyperiodinaneHCID 1512576(R)-N-Boc-2-hydroxymethylmorpholineHCID 5049666Sodium triacetoxyborohydrideHCID 46743200
N-(3,4-dichlorophenyl)piperazine-1-carboxamide hydrochloride

生成物 1

HCID 57656853tert-butyl (2S)-2-[(4-{[(3,4-dichlorophenyl)amino]-carbonyl}piperazin-1-yl)methyl]morpholine-4-carboxylate収率 24.1%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

Dess-Martin periodinane (8.60 g) was added to tert-butyl (2R)-2-(hydroxymethyl)morpholine-4-carboxylate (4.00 g) in dry DCM at 0° C. The reaction was warmed to RT and stirred for a further 2 h. Aqueous sodium thiosulfate (10% w/v, 50 ml) was added and the DCM layer was removed then dried (MgSO4), filtered and evaporated to form the crude aldehyde. The residue was then dissolved in dry dichloromethane (100 ml) followed by addition of N-(3,4-dichlorophenyl)piperazine-1-carboxamide hydrochloride (5.72 g), N, N-diisopropylethylamine (3.17 mL) and NaBH(OAc)3 (9.76 g) and the reaction was stirred under argon for 18 h. 1M NaOH (50 mL) was added followed by vigorous stirring and the dichloromethane layer was extracted. The organic layer was dried (MgSO4), filtered and evaporated. Purification by chromatography (EtOAc neat) afforded the title compound (2.10 g) as a white foam.

後処理

  1. customthe DCM layer was removed
  2. dry with materialthen dried (MgSO4)
  3. filtrationfiltered
  4. customevaporated
  5. customto form the crude aldehyde
  6. stirringthe reaction was stirred under argon for 18 h
  7. stirringby vigorous stirring
  8. extractionthe dichloromethane layer was extracted
  9. dry with materialThe organic layer was dried (MgSO4)
  10. filtrationfiltered
  11. customevaporated
  12. customPurification by chromatography (EtOAc neat)

出典と根拠

ORDレコード
ord-0528fbe1ee724e589af00e0ed62e119d
出典データセット
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08710224B2

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