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Benzenethiol, 2-amino-, hydrochloride (1:1) → Ethyl 2-[4-(benzothiazol-2-yl)methyl-3,4-dihydro-3-oxo-2H-1,4-benzothiazin-2-yl]acetate

HRID 1655894
ノート
印刷プレビュー

反応式

HRID 1655894 の反応式
[C:1]([CH2:3][N:4]1[C:9]2[CH:10]=[CH:11][CH:12]=[CH:13][C:8]=2[S:7][CH:6]([CH2:14][C:15]([O:17][CH2:18][CH3:19])=[O:16])[C:5]1=[O:20])#[N:2].Cl.N[C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][C:24]=1[SH:29]>O>[S:29]1[C:24]2[CH:25]=[CH:26][CH:27]=[CH:28][C:23]=2[N:2]=[C:1]1[CH2:3][N:4]1[C:9]2[CH:10]=[CH:11][CH:12]=[CH:13][C:8]=2[S:7][CH:6]([CH2:14][C:15]([O:17][CH2:18][CH3:19])=[O:16])[C:5]1=[O:20]
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

4

反応物 2

HCID 76794Benzenethiol, 2-amino-, hydrochloride (1:1)HCID 10062806Ethyl 2-(4-cyanomethyl-3,4-dihydro-3-oxo-2H-1,4-benzothiazin-2-yl)acetate

生成物 1

HCID 9978204Ethyl 2-[4-(benzothiazol-2-yl)methyl-3,4-dihydro-3-oxo-2H-1,4-benzothiazin-2-yl]acetate収率 68.7%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
180 °C

実験手順

A mixture of 208 mg of ethyl 2-(4-cyanomethyl-3,4-dihydro-3-oxo-2H-1,4-benzothiazin-2-yl)acetate and 116 mg of 2-aminothiophenol hydrochloride was heated at 180° C. for 15 minutes to fuse them. After the mixture had been cooled, water was added, and then extracted with ethyl acetate. After the drying of the organic layer over anhydrous magnesium sulfate, the solvent was distilled off. The resulting oily matter was purified by silica gel chromatography to give 196 mg of the title compound. The structural formula and physical data of this compound are shown in Table 15.

後処理

  1. temperatureAfter the mixture had been cooled
  2. extractionextracted with ethyl acetate
  3. dry with materialAfter the drying of the organic layer over anhydrous magnesium sulfate
  4. distillationthe solvent was distilled off
  5. customThe resulting oily matter was purified by silica gel chromatography

出典と根拠

ORDレコード
ord-c897ccbf25c14139924b6ecfb0f78c98
出典データセット
uspto-grants-1993_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05252571

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート