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Methylamine → 1,1,1-trifluoro-N-methyl-methanesulfonamide

HRID 349611
ノート
印刷プレビュー

反応式

HRID 349611 の反応式
[CH3:1][NH2:2].[F:3][C:4]([F:10])([F:9])[S:5](F)(=[O:7])=[O:6]>ClCCl>[CH3:1][NH:2][S:5]([C:4]([F:10])([F:9])[F:3])(=[O:7])=[O:6]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 6329Methylamine2 回HCID 67631Methanesulfonyl fluoride, trifluoro-

生成物 1

HCID 124897411,1,1-trifluoro-N-methyl-methanesulfonamide

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A weighed pressure reactor (available from Parr Instrument Co., Moline, Ill.) is charged with dichloromethane (100 mL) and is then cooled using liquid nitrogen. Methylamine is introduced from a cylinder via a stainless steel tube that is connected to a valve on the reactor. The reactor is periodically weighed, and methylamine is added until 20 g have been added. Trifluoromethanesulfonylfluoride is then introduced into the reactor from a cylinder via a stainless steel tube until 97.9 g have been added. The pressure reactor is then sealed and is placed in a motorized rocker and is rocked and allowed to warm to room temperature. After a period of about 6 hours after the reactor reaches room temperature, it is slowly vented to the atmosphere by opening the valve. The product residue is washed with 10 weight percent aqueous HCl and the organic phase is then dried over MgSO4. The mixture is filtered and the solvent is removed from the filtrate using a rotary evaporator to afford the product.

後処理

  1. temperatureis then cooled
  2. customis connected to a valve on the reactor
  3. additionhave been added
  4. additionhave been added
  5. customThe pressure reactor is then sealed
  6. washThe product residue is washed with 10 weight percent aqueous HCl
  7. dry with materialthe organic phase is then dried over MgSO4
  8. filtrationThe mixture is filtered
  9. customthe solvent is removed from the filtrate
  10. customa rotary evaporator
  11. customto afford the product

出典と根拠

ORDレコード
ord-46010472bf9b457698c12b06de3e9adf
出典データセット
uspto-grants-2007_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07179923B2

反応ノート

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