Hydrochloric Acid → HCID 59828832, 화합물

HRID 1190944노트

반응식

HRID 1190944 반응식
[Cl:1][C:2]1[CH:18]=[CH:17][C:5]2[CH2:6][CH2:7][N:8]([C:11](=[O:16])[C:12]([F:15])([F:14])[F:13])[CH2:9][CH2:10][C:4]=2[C:3]=1[NH:19][CH2:20][C:21]1[CH:26]=[CH:25][C:24]([C:27]2([CH3:32])OCC[O:28]2)=[CH:23][CH:22]=1.Cl>CO>[C:27]([C:24]1[CH:23]=[CH:22][C:21]([CH2:20][NH:19][C:3]2[C:4]3[CH2:10][CH2:9][N:8]([C:11](=[O:16])[C:12]([F:14])([F:15])[F:13])[CH2:7][CH2:6][C:5]=3[CH:17]=[CH:18][C:2]=2[Cl:1])=[CH:26][CH:25]=1)(=[O:28])[CH3:32]

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 7-chloro-6-[4-(2-methyl-[1,3]dioxolan-2-yl)-benzylamino]-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 room 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 in vacuo. Purify by chromatography on silica gel eluting with hexane/EtOAc (1:0, 9:1, 17:3 and 4:1) to obtain the title compound as an oil (107 mg, 79%). GC-MS m/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 in vacuo
  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-dc203b743bc945f8a0172f3fdaee8bbc
출처 데이터셋
uspto-grants-2014_03
특허 번호
US08680091B2

반응 노트

불러오는 중…