Hydrochloric Acid → 7-(4-Morpholinophenyl)-2,3-dihydro-1-benzothiepine-4-carboxylic acid

HRID 1388010ノート

反応式

HRID 1388010 の反応式
[O:1]1[CH2:6][CH2:5][N:4]([C:7]2[CH:12]=[CH:11][C:10]([C:13]3[CH:14]=[CH:15][C:16]4[S:22][CH2:21][CH2:20][C:19]([C:23]([O:25]C)=[O:24])=[CH:18][C:17]=4[CH:27]=3)=[CH:9][CH:8]=2)[CH2:3][CH2:2]1.[OH-].[Na+].Cl>C(O)C.C1COCC1>[O:1]1[CH2:2][CH2:3][N:4]([C:7]2[CH:12]=[CH:11][C:10]([C:13]3[CH:14]=[CH:15][C:16]4[S:22][CH2:21][CH2:20][C:19]([C:23]([OH:25])=[O:24])=[CH:18][C:17]=4[CH:27]=3)=[CH:9][CH:8]=2)[CH2:5][CH2:6]1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 18472523Methyl 7-(4-morpholinophenyl)-2,3-dihydro-1-benzothiepine-4-carboxylate

生成物 1

HCID 184722757-(4-Morpholinophenyl)-2,3-dihydro-1-benzothiepine-4-carboxylic acid収率 94.8%

試薬・触媒・溶媒 1

HCID 21873804Tetrahydrofuran ethanol溶媒

実験手順

To a solution of methyl 7-(4-morpholinophenyl)-2,3-dihydro-1-benzothiepine-4-carboxylate (0.55 g) in ethanol/THF (30/30 ml) was added at room temperature 1N sodium hydroxide solution (1.8 ml), and the mixture was stirred for 6 days and then refluxed for 2 hours. To the mixture was added 1N hydrochloric acid (1.8 ml). The resulting solid was collected by filtration, which was washed with ethanol and diethylether to give yellow powder of 7-(4-morpholinophenyl)-2,3-dihydro-l-benzo-thiepine-4-carboxylic acid (502.2 mg).

後処理

  1. temperaturerefluxed for 2 hours
  2. filtrationThe resulting solid was collected by filtration, which
  3. washwas washed with ethanol and diethylether

出典と根拠

ORDレコード
ord-fca14c9856a74457bd3bb7aa9f57bd6e
出典データセット
uspto-grants-2001_07
特許番号
US06268354B1

反応ノート

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