Hydrochloric Acid → [2-(3-Amino-propylamino)-thiazol-5-yl]-o-tolyl-methanone

HRID 2119606ノート

反応式

HRID 2119606 の反応式
C(OC(=O)[NH:7][CH2:8][CH2:9][CH2:10][NH:11][C:12]1[S:13][C:14]([C:17](=[O:25])[C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=2[CH3:24])=[CH:15][N:16]=1)(C)(C)C.Cl.C(=O)(O)[O-].[Na+]>O1CCOCC1>[NH2:7][CH2:8][CH2:9][CH2:10][NH:11][C:12]1[S:13][C:14]([C:17]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=2[CH3:24])=[O:25])=[CH:15][N:16]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 516892Sodium BicarbonateHCID 20616905{3-[5-(2-Methyl-benzoyl)-thiazol-2-ylamino]-propyl}-carbamic Acid tert-butyl Ester

生成物 1

HCID 23442548[2-(3-Amino-propylamino)-thiazol-5-yl]-o-tolyl-methanone収率 102.2%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

339 mg {3-[5-(2-Methyl-benzoyl)-thiazol-2-ylamino]-propyl}-carbamic acid tert-butyl ester was added to a solution of 25% aqueous hydrochloric acid in dioxane. The mixture was stirred 1 h at room temperature and maintained overnight in the refrigerator. The mixture was poured into saturated aqueous sodium bicarbonate solution (50 ml). The organics were extracted with dichloromethane (3×50 ml), dried over magnesium sulfate and evaporated under reduced pressure to afford the title compound as yellow foam (254 mg) which was used without further purification.

後処理

  1. temperaturemaintained overnight in the refrigerator
  2. extractionThe organics were extracted with dichloromethane (3×50 ml)
  3. dry with materialdried over magnesium sulfate
  4. customevaporated under reduced pressure

出典と根拠

ORDレコード
ord-e5002b6f0d2f4f38949d84439ff9188f
出典データセット
uspto-grants-2004_02
特許番号
US06686381B2

反応ノート

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