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Hydrochloric Acid → HCID 57114887, 화합물

HRID 1351892
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HRID 1351892 반응식
[F:1][CH2:2][O:3][C:4]1[CH:33]=[CH:32][C:7]2[CH2:8][CH2:9][CH2:10][CH:11]([N:13](C(OC(C)(C)C)=O)[CH2:14][C@H:15]([OH:24])[CH2:16][O:17][C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)[CH2:12][C:6]=2[CH:5]=1.Cl.C(=O)([O-])O.[Na+]>C(OCC)(=O)C>[F:1][CH2:2][O:3][C:4]1[CH:33]=[CH:32][C:7]2[CH2:8][CH2:9][CH2:10][CH:11]([NH:13][CH2:14][C@H:15]([OH:24])[CH2:16][O:17][C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)[CH2:12][C:6]=2[CH:5]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 516892Sodium Bicarbonate2회HCID 56978727HCID 56978727, 화합물

생성물 1

HCID 57114887HCID 57114887, 화합물수율 71.7%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매3회

실험 절차

To a solution of N-(3-fluoromethoxy-6,7,8,9-tetrahydro-5H-benzocyclohepten-6-yl)-N-[(2S)-2-hydroxy-3-phenoxypropyl]-tert-butoxycarbonylamine (41 mg) in ethyl acetate (2 ml) was added 4N hydrogen chloride in ethyl acetate (0.45 ml) at room temperature, and the mixture was stirred at the same temperature for 5.5 hours. The mixture was poured into a mixture of saturated aqueous sodium hydrogencarbonate and ethyl acetate, followed by being made basic with saturated aqueous sodium hydrogencarbonate. After separation, the organic layer was dried over anhydrous magnesium sulfate and evaporated in vacuo. The residue was purified by preparative thin layer chromatography (silica gel, chloroform:methanol=10:1) to give (2S)-1-(3-fluoromethoxy-6,7,8,9-tetrahydro-5H-benzocyclohepten-6-yl)amino-3-phenoxy-2-propanol (23 mg).

후처리

  1. customAfter separation
  2. dry with materialthe organic layer was dried over anhydrous magnesium sulfate
  3. customevaporated in vacuo
  4. customThe residue was purified by preparative thin layer chromatography (silica gel, chloroform:methanol=10:1)

출처 및 근거

ORD 기록
ord-1ac2766e93154d61a5c4d6ac644d674e
출처 데이터셋
uspto-grants-2007_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07217706B2

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