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

HRID 566080노트

반응식

HRID 566080 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 21873804Tetrahydrofuran ethanol용매

실험 절차

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-1-benzo-thiepine-4-carboxylic acid (502.2 mg).

후처리

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

출처 및 근거

ORD 기록
ord-eb40cbd0441b4fe5bc7713156119c134
출처 데이터셋
uspto-grants-2001_01
특허 번호
US06172061B2

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