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

Aldoxime → 4-chloro-2-(ethoxymethyl)-1-[2-(3-methyl-1-oxa-2,4-diazaspiro[4,4]non-2-en-4-yl)ethyl]-1H-imidazo[4,5-c]quinoline

HRID 606084
ノート
印刷プレビュー

反応式

HRID 606084 の反応式
[Cl:1][C:2]1[C:11]2[N:12]=[C:13]([CH2:18][O:19][CH2:20][CH3:21])[N:14]([CH2:15][CH2:16][NH2:17])[C:10]=2[C:9]2[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=2[N:3]=1.[C:22]1(=[O:27])[CH2:26][CH2:25][CH2:24][CH2:23]1.S([O-])([O-])(=O)=O.[Mg+2].[CH:34](=[N:36]O)[CH3:35].ClN1C(=O)CCC1=O.C(N(CC)CC)C>ClCCl>[Cl:1][C:2]1[C:11]2[N:12]=[C:13]([CH2:18][O:19][CH2:20][CH3:21])[N:14]([CH2:15][CH2:16][N:17]3[C:22]4([CH2:26][CH2:25][CH2:24][CH2:23]4)[O:27][N:36]=[C:34]3[CH3:35])[C:10]=2[C:9]2[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=2[N:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 6

HCID 7863AldoximeHCID 8452CyclopentanoneHCID 8471TriethylamineHCID 24083Sulfuric acid magnesium salt (1:1)HCID 31398ChlorosuccinimideHCID 862476222-(4-chloro-2-ethoxymethyl-1H-imidazo[4,5-c]quinolin-1-yl)ethylamine

生成物 1

HCID 86616887
4-chloro-2-(ethoxymethyl)-1-[2-(3-methyl-1-oxa-2,4-diazaspiro[4,4]non-2-en-4-yl)ethyl]-1H-imidazo[4,5-c]quinoline
収率 54.9%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A mixture of 2-(4-chloro-2-ethoxymethyl-1H-imidazo[4,5-c]quinolin-1-yl)ethylamine (1.00 g, 3.28 mmol), cyclopentanone (0.32 mL, 3.6 mmol), and magnesium sulfate in dichloromethane was stirred at room temperature overnight. The mixture was filtered and the filtrate was concentrated under reduced pressure. The residue was dissolved in dichloromethane (20 mL) along with N-hydroxyethanimidoyl chloride, which was prepared from acetaldehyde oxime (242 mg, 4.10 mmol) and N-chlorosuccinimide (537 mg, 4.10 mmol) according to the method described in Part G of Example 10. The resulting solution was cooled in an ice bath and triethylamine (0.69 mL, 4.9 mmol) was added. The mixture was allowed to warm slowly to room temperature and stirred overnight. The work-up and purification procedures described in Part G of Example 10 were followed to provide 770 mg of 4-chloro-2-(ethoxymethyl)-1-[2-(3-methyl-1-oxa-2,4-diazaspiro[4,4]non-2-en-4-yl)ethyl]-1H-imidazo[4,5-c]quinoline as a clear, colorless oil.

後処理

  1. filtrationThe mixture was filtered
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. dissolutionThe residue was dissolved in dichloromethane (20 mL) along with N-hydroxyethanimidoyl chloride, which
  4. temperatureThe resulting solution was cooled in an ice bath
  5. temperatureto warm slowly to room temperature
  6. stirringstirred overnight
  7. customThe work-up and purification procedures

出典と根拠

ORDレコード
ord-70ff8d3d1cae4c6dbf645630c8096baa
出典データセット
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07915281B2

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