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Hydrochloric Acid → 7-sulfamoyl-3,4-dihydrothieno[3,2-f]-1,4-thiazepin-5(2H)-one

HRID 1197428
ノート
印刷プレビュー

反応式

HRID 1197428 の反応式
[Na].[NH2:2][CH2:3][CH2:4][SH:5].Cl[C:7]1[S:11][C:10]([S:12]([NH2:15])(=[O:14])=[O:13])=[CH:9][C:8]=1[C:16](OCC)=[O:17].Cl>C(O)C>[S:12]([C:10]1[S:11][C:7]2[S:5][CH2:4][CH2:3][NH:2][C:16](=[O:17])[C:8]=2[CH:9]=1)(=[O:14])(=[O:13])[NH2:15]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 6058CysteamineHCID 5360545Sodium2 回HCID 19106450Ethyl 2-chloro-5-sulfamoylthiophene-3-carboxylate

生成物 1

HCID 191064767-sulfamoyl-3,4-dihydrothieno[3,2-f]-1,4-thiazepin-5(2H)-one

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a round bottomed flask were added ethanol (200 mL) followed by solid sodium (1.0 g, 43.5 mmole). After the sodium dissolved, 2-aminoethanethiol was added (1.57 g, 20.4 mmole). The reaction was stirred for approximately 5.0 minutes and 5-chloro-4-carboethoxythiophene-2-sulfonamide (5.0 g, 18.5 mmole) was added. The reaction was heated at reflux for 24 hrs. The cooled reaction mixture was acidified (6.0N HCl) and the solvent was removed under vacuum. The residue was triturated with water and the resulting solid collected: 4.77 g (98%) mp>270° C.

後処理

  1. temperatureThe reaction was heated
  2. temperatureat reflux for 24 hrs
  3. customThe cooled reaction mixture
  4. customthe solvent was removed under vacuum
  5. customThe residue was triturated with water
  6. customthe resulting solid collected

出典と根拠

ORDレコード
ord-92ea9783b6a44c5b87d9308cc48e1c23
出典データセット
uspto-grants-1994_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05276025

反応ノート

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