Hydrochloric Acid → HCID 59828832, 화합물

HRID 911366노트

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HRID 911366 반응식
[CH3:1][C:2]1([C:7]2[CH:32]=[CH:31][C:10]([CH2:11][NH:12][C:13]3[C:23]4[CH2:22][CH2:21][N:20]([C:24](=[O:29])[C:25]([F:28])([F:27])[F:26])[CH2:19][CH2:18][C:17]=4[CH:16]=[CH:15][C:14]=3[Cl:30])=[CH:9][CH:8]=2)OCC[O:3]1.Cl>CO>[C:2]([C:7]1[CH:8]=[CH:9][C:10]([CH2:11][NH:12][C:13]2[C:23]3[CH2:22][CH2:21][N:20]([C:24](=[O:29])[C:25]([F:27])([F:28])[F:26])[CH2:19][CH2:18][C:17]=3[CH:16]=[CH:15][C:14]=2[Cl:30])=[CH:31][CH:32]=1)(=[O:3])[CH3:1]

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 59828873HCID 59828873, 화합물

생성물 1

HCID 59828832HCID 59828832, 화합물수율 79%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Dissolve 6-{4-(2-methyl-[1,3]dioxolan-2-yl)benzylamino}-7-chloro-3-(2,2,2-trifluoroacetyl)-2,3,4,5-tetrahydro-1H-benzo[d]azepine (150 mg, 0.32 mmol) in methanol (5 mL) and add 1N aqueous HCl (1 mL). Stir the solution at ambient temperature for 2 h. Remove the solvent, dissolve the residue in DCM and wash with saturated aqueous NaHCO3. Dry the organic phase over Na2SO4, filter and concentrate. Purify by chromatography on silica gel eluting with hexane/EtOAc (1:0, 9:1, 17:3 and 4:1) to obtain 6-(4-acetyl-benzylamino)-7-chloro-3-(2,2,2-trifluoroacetyl)-2,3,4,5-tetrahydro-1H-benzo[d]azepine as an oil (107 mg, 79%). GC-MS m/z/z 424 (M+).

후처리

  1. customRemove the solvent
  2. dissolutiondissolve the residue in DCM
  3. washwash with saturated aqueous NaHCO3
  4. dry with materialDry the organic phase over Na2SO4
  5. filtrationfilter
  6. concentrationconcentrate
  7. customPurify by chromatography on silica gel eluting with hexane/EtOAc (1:0, 9:1, 17:3 and 4:1)

출처 및 근거

ORD 기록
ord-e677e2fcda29455cb114b361a732a963
출처 데이터셋
uspto-grants-2011_09
특허 번호
US08022062B2

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