Potassium Carbonate → Ethyl (N-methyl-3-trifluoromethylbenzylsulfonamido)acetate

HRID 476519

反応式

HRID 476519 の反応式
[F:1][C:2]([F:15])([F:14])[C:3]1[CH:4]=[C:5]([CH:11]=[CH:12][CH:13]=1)[CH2:6][S:7](Cl)(=[O:9])=[O:8].[CH2:16]([O:18][C:19](=[O:23])[CH2:20][NH:21][CH3:22])[CH3:17].C(=O)([O-])[O-].[K+].[K+]>O>[CH3:22][N:21]([CH2:20][C:19]([O:18][CH2:16][CH3:17])=[O:23])[S:7]([CH2:6][C:5]1[CH:11]=[CH:12][CH:13]=[C:3]([C:2]([F:15])([F:14])[F:1])[CH:4]=1)(=[O:9])=[O:8]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 95849Glycine, N-methyl-, ethyl esterHCID 27946463-(Trifluoromethyl)phenylmethanesulfonyl chloride

生成物 1

HCID 15118078Ethyl (N-methyl-3-trifluoromethylbenzylsulfonamido)acetate

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
70 °C

実験手順

In this example, 22 g of 3-trifluoromethylbenzylsulfonyl chloride was added cautiously to a solution containing 27 g of the hydrochloride salt of sarcosine ethyl ester and 12 g of potassium carbonate in 90 ml of water at room temperature. The reaction mixture was heated to about 70° C. and maintained at this temperature for about four hours. The mixture was allowed to cool and then extracted with ethyl ether. The ethyl ether extract was dried over magnesium sulfate, filtered, and evaporated to dryness yielding 9.5 g of the title compound as an off-white solid.

後処理

  1. temperaturemaintained at this temperature for about four hours
  2. temperatureto cool
  3. extractionextracted with ethyl ether
  4. extractionThe ethyl ether extract
  5. dry with materialwas dried over magnesium sulfate
  6. filtrationfiltered
  7. customevaporated to dryness

出典と根拠

ORDレコード
ord-83bc17cc94464749af416e1a13827d0e
出典データセット
uspto-grants-1989_12
特許番号
US04885027

関連ノート

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