Water → 3-Chloro-4-(1,1-dioxo-[1,2]thiazinan-2-yl)-toluene

HRID 2094299

反応式

HRID 2094299 の反応式
[Cl:1][C:2]1[CH:16]=[C:15]([CH3:17])[CH:14]=[CH:13][C:3]=1[NH:4][S:5]([CH2:8][CH2:9][CH2:10][CH2:11]Cl)(=[O:7])=[O:6].[K].CC(C)([O-])C.O>CN(C=O)C>[Cl:1][C:2]1[CH:16]=[C:15]([CH3:17])[CH:14]=[CH:13][C:3]=1[N:4]1[CH2:11][CH2:10][CH2:9][CH2:8][S:5]1(=[O:7])=[O:6]

参加物

5

反応物 3

HCID 962WaterHCID 50987170Potassium tertbutoxideHCID 670486822-chloro-N-(4-chlorobutyl-sulphonyl)-4-methyl-aniline

生成物 1

HCID 667317213-Chloro-4-(1,1-dioxo-[1,2]thiazinan-2-yl)-toluene

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

1.27 g (4.29 mmol) 2-chloro-N-(4-chlorbutyl-sulphonyl)-4-methyl-aniline are stirred together with 722 mg (6.43 mmol) potassium-tert.-butoxide in 50 ml DMF for 16 hours at 60° C. Then the reaction mixture is poured into water and extracted with ethyl acetate. The combined organic phases are dried over sodium sulphate and evaporated down i. vac. The residue is purified by chromatography on silica gel (eluant: petroleum ether/ethyl acetate=3:2).

後処理

  1. extractionextracted with ethyl acetate
  2. dry with materialThe combined organic phases are dried over sodium sulphate
  3. customevaporated down i
  4. customThe residue is purified by chromatography on silica gel (eluant: petroleum ether/ethyl acetate=3:2)

出典と根拠

ORDレコード
ord-4a2b9096f60248988f35e97002aefd5d
出典データセット
uspto-grants-2013_05
特許番号
US08445525B2

関連ノート

読み込み中…