Hydrochloric Acid → 3-Methyl-1-benzothiophen-2-amine hydrochloride

HRID 1691572

反応式

HRID 1691572 の反応式
[ClH:1].C(OC(=O)[NH:8][C:9]1[S:13][C:12]2[CH:14]=[CH:15][CH:16]=[CH:17][C:11]=2[C:10]=1[CH3:18])(C)(C)C>O1CCOCC1>[ClH:1].[CH3:18][C:10]1[C:11]2[CH:17]=[CH:16][CH:15]=[CH:14][C:12]=2[S:13][C:9]=1[NH2:8]

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 57920379Tert-butyl-3-methylbenzo[b]thiophen-2-ylcarbamate

生成物 1

HCID 567239383-Methyl-1-benzothiophen-2-amine hydrochloride

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

反応条件

温度
22 °C

実験手順

A 5-L 3-neck flask equipped with an overhead mechanical stirrer, N2 inlet/outlet adapter, and thermocouple was charged with 4M HCl in dioxane (3.1 L), compound 306-B (265 g, 1.0 mol) and stirred for 18 h at 22° C. The white precipitate was collected by filtration, washed with diethyl ether (3×500 mL), and dried under house vacuum at 40° C. for 48 h to afford 174 g of compound 757-A as a white solid. 1H-NMR (DMSO-d6): δ 8.7 (br s, 3H), 7.71 (d, 1H), 7.44 (d, 1H), 7.29 (t, 1H), 7.14 (t, 1H), 2.184 (s, 3H).

後処理

  1. customA 5-L 3-neck flask equipped with an overhead mechanical stirrer, N2 inlet/outlet adapter
  2. filtrationThe white precipitate was collected by filtration
  3. washwashed with diethyl ether (3×500 mL)
  4. customdried under house vacuum at 40° C. for 48 h

出典と根拠

ORDレコード
ord-8ff62a1c9d6d4139a8c7fb736ea62606
出典データセット
uspto-grants-2012_04
特許番号
US08153682B2

関連ノート

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