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Hydrochloric Acid → HCID 22615054, 화합물

HRID 843156
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HRID 843156 반응식
C([O:3][C:4]([C:6]1[O:7][C:8]2[CH:15]=[CH:14][CH:13]=[C:12]([O:16][CH2:17][CH:18]([OH:24])[CH2:19][NH:20][CH:21]([CH3:23])[CH3:22])[C:9]=2[C:10]=1[CH3:11])=[O:5])C.[OH-].[Na+].Cl>CO>[OH:24][CH:18]([CH2:19][NH:20][CH:21]([CH3:23])[CH3:22])[CH2:17][O:16][C:12]1[C:9]2[C:10]([CH3:11])=[C:6]([C:4]([OH:5])=[O:3])[O:7][C:8]=2[CH:15]=[CH:14][CH:13]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 489104HCID 489104, 화합물

생성물 1

HCID 22615054HCID 22615054, 화합물수율 86.2%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A solution of 4-(2-hydroxy-3-isopropylamino-propoxy)-3-methyl-benzofuran-2-carboxylic acid ethyl ester (100 mg) in methanol (5 ml) was treated with 5 N NaOH solution (1 ml) at room temperature, and the resulting mixture was stirred overnight at the same temperature. The solution was acidified with 1N HCl solution (6 ml) and concentrated in vacuo. The residue was dissolved in H2O and passed through Sep-Pak Cartridge (C18) which was developed with H2O-MeOH. The fractions containing the target compound were collected and concentrated in vacuo to give 4-(2-hydroxy-3-isopropylamino-propoxy)-3-methyl-benzofuran-2-carboxylic acid (79 mg) as a white powder. FAB-MS: m/z 308 (MH+); 1H-NMR (DMSO-d6): δ 1.05 (6H, d, J=6 Hz), 2.65 (3H, s), 2.73 (1H, dd, J1=12 Hz, J2=7 Hz), 2.86 (2H, m), 3.99 (1H, m), 4.16 (2H, d, J=5 Hz), 6.68 (1H, d, J=8 Hz), 7.01 (1H, d, J=8 Hz), 7.17 (1H, t, J=8 Hz).

후처리

  1. concentrationconcentrated in vacuo
  2. dissolutionThe residue was dissolved in H2O
  3. additionThe fractions containing the target compound
  4. customwere collected
  5. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-a0be45c60cb948dd99426a866fa1e1ce
출처 데이터셋
uspto-grants-2002_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06376491B1

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