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Sodium Hydroxide → (2-(5-Chloro-2-methoxybenzoylamino)ethyl]-5-(methylaminocarbonylaminosulfonyl)thiophene

HRID 482022
ノート
印刷プレビュー

反応式

HRID 482022 の反応式
[OH-].[Na+].[CH3:3][NH:4][C:5](=[O:10])C(Cl)(Cl)Cl.[Cl:11][C:12]1[CH:13]=[CH:14][C:15]([O:32][CH3:33])=[C:16]([CH:31]=1)[C:17]([NH:19][CH2:20][CH2:21][C:22]1[S:23][C:24]([S:27](=[O:30])(=[O:29])[NH2:28])=[CH:25][CH:26]=1)=[O:18]>CS(C)=O>[Cl:11][C:12]1[CH:13]=[CH:14][C:15]([O:32][CH3:33])=[C:16]([CH:31]=1)[C:17]([NH:19][CH2:20][CH2:21][C:22]1[S:23][C:24]([S:27]([NH:28][C:5]([NH:4][CH3:3])=[O:10])(=[O:29])=[O:30])=[CH:25][CH:26]=1)=[O:18]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 2486522,2,2-Trichloro-n-methylacetamideHCID 152886722-[2-(5-Chloro-2-methoxybenzoylamino)ethyl]-5-sulfamoylthiophene

生成物 1

HCID 9802837(2-(5-Chloro-2-methoxybenzoylamino)ethyl]-5-(methylaminocarbonylaminosulfonyl)thiophene

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

反応条件

温度
65 °C

実験手順

120 mg of powdered NaOH and 141 mg of N-methyltrichloro-acetamide (0.8 mmol) were added to 299 mg (0.8 mmol) of 2-[2-(5-chloro-2-methoxybenzoylamino)ethyl]-5-sulfamoyl-thiophene in 9 ml of DMSO. The mixture was stir 65° C. for 1.5 hours. After cooling, it was stirred into ice water of pH 2. The precipitate was filtered off with suction and taken up in CH2Cl2, and the solution was washed with water and dried using MgSO4. After evaporating the solvent, a yellow-brown crude product remained which, after treatment with CH2Cl2 /5% methanol, crystallized at -4° C.

後処理

  1. temperatureAfter cooling
  2. filtrationThe precipitate was filtered off with suction
  3. washthe solution was washed with water
  4. customdried
  5. customAfter evaporating the solvent
  6. customafter treatment with CH2Cl2 /5% methanol, crystallized at -4° C.

出典と根拠

ORDレコード
ord-16b3842ff8724a55bc81d390fd245322
出典データセット
uspto-grants-1998_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05792788

反応ノート

読み込み中…

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