Triethylamine → N-cyclopropyl-3-trifluoromethylbenzylsulfonamide

HRID 476522

反応式

HRID 476522 の反応式
[CH:1]1([NH2:4])[CH2:3][CH2:2]1.C(N(CC)CC)C.[F:12][C:13]([F:26])([F:25])[C:14]1[CH:15]=[C:16]([CH:22]=[CH:23][CH:24]=1)[CH2:17][S:18](Cl)(=[O:20])=[O:19]>C(Cl)Cl>[CH:1]1([NH:4][S:18]([CH2:17][C:16]2[CH:22]=[CH:23][CH:24]=[C:14]([C:13]([F:12])([F:25])[F:26])[CH:15]=2)(=[O:20])=[O:19])[CH2:3][CH2:2]1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 69828CyclopropylamineHCID 27946463-(Trifluoromethyl)phenylmethanesulfonyl chloride

生成物 1

HCID 15615994N-cyclopropyl-3-trifluoromethylbenzylsulfonamide収率 92.6%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

In this example, 5.3 g of cyclopropylamine is mixed with 9.4 g of triethylamine and then added dropwise to a solution containing 20 g of 3-trifluoromethylbenzylsulfonyl chloride in methylene chloride at 0° C. The resulting reaction mixture is stirred at room temperature (i.e., about 20°-25° C.) for 3 hours. The reaction mixture is washed with saturated aqueous ammonium chloride and then with aqueous 1 wt.% hydrochloric acid until it was neutral. The organic layer is separated, washed twice with 50 ml of aqueous saturated sodium chloride solution, dried over magnesium sulfate and then evaporated to dryness affording 20 g of N-cyclopropyl-3-trifluoromethylbenzylsulfonamide.

後処理

  1. additionadded dropwise to a solution
  2. customThe resulting reaction mixture
  3. washThe reaction mixture is washed with saturated aqueous ammonium chloride
  4. customThe organic layer is separated
  5. washwashed twice with 50 ml of aqueous saturated sodium chloride solution
  6. dry with materialdried over magnesium sulfate
  7. customevaporated to dryness

出典と根拠

ORDレコード
ord-8c78722a0a994ec08124fa80042d3719
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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