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

Dimethylformamide → N-(2-Amino-1-cyano-2-oxoethyl)-5-chloro-6-[4-(2-oxo-2H-3,1-benzoxazin-1(4H)-yl)piperidin-1-yl]pyridine-3-carboxamide

HRID 2414339
ノート
印刷プレビュー

反応式

HRID 2414339 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([C:25](O)=[O:26])[CH:5]=[N:6][C:7]=1[N:8]1[CH2:13][CH2:12][CH:11]([N:14]2[C:19]3[CH:20]=[CH:21][CH:22]=[CH:23][C:18]=3[CH2:17][O:16][C:15]2=[O:24])[CH2:10][CH2:9]1.C(Cl)(=O)C(Cl)=O.C[N:35](C)[CH:36]=[O:37].C([N:42](CC)[CH:43]([CH3:45])C)(C)C.C[N:49]1CCCC1=O>ClCCl>[NH2:35][C:36](=[O:37])[CH:45]([NH:49][C:25]([C:4]1[CH:5]=[N:6][C:7]([N:8]2[CH2:13][CH2:12][CH:11]([N:14]3[C:19]4[CH:20]=[CH:21][CH:22]=[CH:23][C:18]=4[CH2:17][O:16][C:15]3=[O:24])[CH2:10][CH2:9]2)=[C:2]([Cl:1])[CH:3]=1)=[O:26])[C:43]#[N:42]
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 6228DimethylformamideHCID 13387N-methyl-2-pyrrolidoneHCID 65578Oxalyl chlorideHCID 81531DiisopropylethylamineHCID 226445845-Chloro-6-[4-(2-oxo-2h-3,1-benzoxazin-1(4h)-yl)piperidin-1-yl]pyridine-3-carboxylic acid

生成物 1

HCID 22644626
N-(2-Amino-1-cyano-2-oxoethyl)-5-chloro-6-[4-(2-oxo-2H-3,1-benzoxazin-1(4H)-yl)piperidin-1-yl]pyridine-3-carboxamide

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

The product of example 148 step (i) (0.14 g) was stirred as a suspension in dichloromethane (4 ml) and to this mixture was added oxalyl chloride (0.05 g) followed by N,N-dimethylformamide (0.01 g). After stirring for 1 h at room temperature the mixture was treated with 2-aminocyanoacetanide (0.14 g) 1-methyl-2-pyrrolidinone (3 ml) and then N,N-diisopropylethylamine (1 ml), stirring was then continued for a further 18 h at room temperature. The reaction mixture was partitioned between aqueous sodium bicarbonate and ethyl acetate, the organic layer was washed with water, dried and evaporated under reduced pressure. Purification was by chromatography eluting with 25% ethyl acetate/isohexane. Yield 0.09 g as a solid.

後処理

  1. waitwas then continued for a further 18 h at room temperature
  2. customThe reaction mixture was partitioned between aqueous sodium bicarbonate and ethyl acetate
  3. washthe organic layer was washed with water
  4. customdried
  5. customevaporated under reduced pressure
  6. customPurification
  7. washeluting with 25% ethyl acetate/isohexane

出典と根拠

ORDレコード
ord-e81565842d6f45cb973086b00fe0a1d1
出典データセット
uspto-grants-2004_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06812226B2

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