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

Oxalyl chloride → 2-Trifluoromethylbenzylsulfonyl chloride

HRID 225984
ノート
印刷プレビュー

反応式

HRID 225984 の反応式
[F:1][C:2]([F:15])([F:14])[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[CH2:9][S:10](O)(=[O:12])=[O:11].C(Cl)(=O)C([Cl:19])=O>C1COCC1.CN(C=O)C>[F:1][C:2]([F:15])([F:14])[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[CH2:9][S:10]([Cl:19])(=[O:12])=[O:11]
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 2

HCID 65578Oxalyl chlorideHCID 86065127HCID 86065127、化合物

生成物 1

HCID 27614532-Trifluoromethylbenzylsulfonyl chloride収率 87.5%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

To a suspension of (2-trifluoromethylphenyl)methanesulfonic acid (20.3 g, 84 mmol) in THF (1.9 L) and DMF (5.0 mL) at −20° C. was added oxalyl chloride (44.7 mL, 0.5 mol) slowly dropwise over 1 hr. The bath temperature was maintained below 0° C. for 4 h, at which point the reaction was evaporated to a volume of ˜250 mL and diluted with 500 mL of ethyl acetate. This solution was washed with brine in a separatory funnel and dried over magnesium sulfate. The solution was then evaporated to a brown oil. This oil was taken up in 500 mL of pet ether (30-50°) and heated with a heat gun until the oil went into solution. The solution was then placed into a dry-ice acetone bath to cool resulting in formation of a white crystalline material. This material was collected via filtration and dried to afford 19 g (85%) of (2-trifluoromethylphenyl)methanesulfonyl chloride as a white solid.

後処理

  1. temperatureThe bath temperature was maintained below 0° C. for 4 h, at which
  2. customwas evaporated to a volume of ˜250 mL
  3. additiondiluted with 500 mL of ethyl acetate
  4. washThis solution was washed with brine in a separatory funnel
  5. dry with materialdried over magnesium sulfate
  6. customThe solution was then evaporated to a brown oil
  7. customwas taken up in 500 mL of pet ether (30-50°)
  8. temperatureheated with a heat gun until the oil
  9. customThe solution was then placed into a dry-ice acetone bath
  10. temperatureto cool
  11. customresulting in formation of a white crystalline material
  12. filtrationThis material was collected via filtration
  13. customdried

出典と根拠

ORDレコード
ord-cd94becf0cef4daa810dc654ef725589
出典データセット
uspto-grants-2009_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07557135B2

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