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

Sulfuric Acid → Diethyl (2,3-dichloro-4,5-difluorobenzoyl)propanedioate

HRID 2232632
ノート
印刷プレビュー

反応式

HRID 2232632 の反応式
[Mg].[C:2]([O:10][CH2:11][CH3:12])(=[O:9])[CH2:3][C:4]([O:6][CH2:7][CH3:8])=[O:5].[Cl:13][C:14]1[C:22]([Cl:23])=[C:21]([F:24])[C:20]([F:25])=[CH:19][C:15]=1[C:16](Cl)=[O:17].S(=O)(=O)(O)O>C1(C)C=CC=CC=1.C(O)C.C(Cl)(Cl)(Cl)Cl>[Cl:13][C:14]1[C:22]([Cl:23])=[C:21]([F:24])[C:20]([F:25])=[CH:19][C:15]=1[C:16]([CH:3]([C:4]([O:6][CH2:7][CH3:8])=[O:5])[C:2]([O:10][CH2:11][CH3:12])=[O:9])=[O:17]
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 4

HCID 1118Sulfuric AcidHCID 7761Diethyl MalonateHCID 5462224MagnesiumHCID 10999320Benzoyl chloride, 2,3-dichloro-4,5-difluoro-

生成物 1

HCID 14071801Diethyl (2,3-dichloro-4,5-difluorobenzoyl)propanedioate収率 107.3%

試薬・触媒・溶媒 3

HCID 702Ethanol
溶媒
2 回
HCID 1140Toluene溶媒2 回
HCID 5943Carbon Tetrachloride溶媒

実験手順

Magnesium turnings (0.77 g) and carbon tetrachloride (0.4 ml) was added to absolute ethanol (5.3 ml). To the stirring suspension was added a solution of diethyl malonate (4.89 g) and absolute ethanol (8.5 ml) in toluene (21.3 ml) dropwise during 40 minutes at 20° to 40° C. The mixture was stirred at 50° to 60° C. for 2 hours, and then cooled in an acetone-dry ice bath. A solution of 2,3-dichloro-4,5-difluorobenzoyl chloride (6.00 g) in anhydrous toluene (7.1 ml) was added dropwise to the resulting solution at -18° to -13° C. during 10 minutes. The mixture was warmed gradually to room temperature during 2 hours and then mixed with ice water (17 ml) containing concentrated sulfuric acid (1.1 ml). The resulting organic layer was collected and the water layer was extracted with toluene. The combined organic layer was washed with water, dried over anhydrous sodium sulfate and then concentrated to give the title compound (9.68 g) as pale yellow oil.

後処理

  1. temperaturecooled in an acetone-dry ice bath
  2. customThe resulting organic layer was collected
  3. extractionthe water layer was extracted with toluene
  4. washThe combined organic layer was washed with water
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-bf7c0540b87742ffbc083bbae5ab2b3d
出典データセット
uspto-grants-1988_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04788320

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