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 → HCID 86621080、化合物

HRID 900756
ノート
印刷プレビュー

反応式

HRID 900756 の反応式
C(Cl)(=O)C(Cl)=O.[Cl:7][C:8]1[N:9]=[C:10]([CH3:37])[N:11]([CH2:14][C:15]2[S:30][C:18]3[N:19]([CH2:26][CH:27]([CH3:29])[CH3:28])[C:20](=[O:25])[N:21]([CH3:24])[C:22](=[O:23])[C:17]=3[C:16]=2[C:31]([N:33]([O:35]C)[CH3:34])=[O:32])[C:12]=1[Cl:13].CN(C)C=O>ClCCl>[Cl:7][C:8]1[N:9]=[C:10]([CH3:37])[N:11]([CH2:14][C:15]2[S:30][C:18]3[N:19]([CH2:26][CH:27]([CH3:29])[CH3:28])[C:20](=[O:25])[N:21]([CH3:24])[C:22](=[O:23])[C:17]=3[C:16]=2[C:31]([N:33]([OH:35])[CH3:34])=[O:32])[C:12]=1[Cl:13]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6228DimethylformamideHCID 65578Oxalyl chlorideHCID 10184774HCID 10184774、化合物

生成物 1

HCID 86621080HCID 86621080、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Oxalyl chloride (0.1 62 ml) was added to a stirred solution of the product of example 1 part d) (415 mg) and dimethylformamide (0.01 ml) in dichloromethane (4 ml). After 1 h the solution was evaporated under reduced pressure. The residue was dissolved in anhydrous tetrahydrofuran (3 ml) and 1 ml of the solution was added to a stirred solution of N-methylhydroxylamine hydrochloride (129 mg) in saturated aqueous sodium bicarbonate solution (2 ml). After 1 h, the mixture was diluted with water (10 ml) and extracted with ethyl acetate (3×10 ml). Organic extracts were dried over anhydrous magnesium sulfate, filtered and evaporated under reduced pressure to give the sub-title compound (129 mg).

後処理

  1. customAfter 1 h the solution was evaporated under reduced pressure
  2. dissolutionThe residue was dissolved in anhydrous tetrahydrofuran (3 ml)
  3. addition1 ml of the solution was added to a stirred solution of N-methylhydroxylamine hydrochloride (129 mg) in saturated aqueous sodium bicarbonate solution (2 ml)
  4. additionthe mixture was diluted with water (10 ml)
  5. extractionextracted with ethyl acetate (3×10 ml)
  6. dry with materialOrganic extracts were dried over anhydrous magnesium sulfate
  7. filtrationfiltered
  8. customevaporated under reduced pressure

出典と根拠

ORDレコード
ord-b79732dfab45459dbeab391ea5900b67
出典データセット
uspto-grants-2008_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07361660B2

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