Triethylamine → 4-[(2-Sulfamoyl-5-thienyl)sulfonyl]phenyl 1-acetylpiperidine-4-carboxylate

HRID 1632742

反応式

HRID 1632742 の反応式
[OH:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([C:11]2[S:15][C:14]([S:16]([NH2:19])(=[O:18])=[O:17])=[CH:13][CH:12]=2)(=[O:10])=[O:9])=[CH:4][CH:3]=1.C(N(CC)CC)C.Cl.[C:28]([N:31]1[CH2:36][CH2:35][CH:34]([C:37](Cl)=[O:38])[CH2:33][CH2:32]1)(=[O:30])[CH3:29]>CC(C)=O>[C:28]([N:31]1[CH2:32][CH2:33][CH:34]([C:37]([O:1][C:2]2[CH:7]=[CH:6][C:5]([S:8]([C:11]3[S:15][C:14]([S:16](=[O:17])(=[O:18])[NH2:19])=[CH:13][CH:12]=3)(=[O:9])=[O:10])=[CH:4][CH:3]=2)=[O:38])[CH2:35][CH2:36]1)(=[O:30])[CH3:29]

参加物

5

反応物 3

HCID 8471Triethylamine3 回HCID 127368925-(4-Hydroxyphenyl)sulfonylthiophene-2-sulfonamideHCID 534308101-Acetylpiperidine-4-carbonyl chloride hydrochloride2 回

生成物 1

HCID 204423674-[(2-Sulfamoyl-5-thienyl)sulfonyl]phenyl 1-acetylpiperidine-4-carboxylate

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

A solution of 5-[(4-hydroxyphenyl)sulfonyl]thiophene-2-sulfonamide (3.19 g; 0.01 mole) in acetone (60 ml) at -15° was treated with triethylamine (1.11 g; 0.011 mole). Then 1-acetylpiperidine-4-carbonyl chloride hydrochloride (2.41 g; 0.011 mole) was added, portionwise, during 15 minutes at -15°. The cooling bath was removed and stirring was continued. After 20 hours at room temperature, the reaction mixture was treated with triethylamine (1.11 g; 0.011 mole). Then after stirring one hour longer, the reaction mixture was treated with 1-acetylpiperidine-4-carbonyl chloride hydrochloride (2.41 g; 0.011 mole) and triethylamine (2.22 g; 0.022 mole) and stirred at room temperature.

後処理

  1. customThe cooling bath was removed
  2. waitAfter 20 hours at room temperature
  3. stirringThen after stirring one hour longer
  4. stirringstirred at room temperature

出典と根拠

ORDレコード
ord-d259bbaad2a743b2b218fca536653630
出典データセット
uspto-grants-1984_10
特許番号
US04477466

関連ノート

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