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Hydrochloric Acid → HCID 19784136, 화합물

HRID 257267
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HRID 257267 반응식
[CH2:1]([C:3]1[N:4]=[C:5]2[C:10]([CH3:11])=[CH:9][C:8]([CH3:12])=[N:7][N:6]2[C:13]=1[CH2:14][C:15]1[CH:33]=[CH:32][C:18]([O:19][CH:20]([C:25]2[CH:30]=[CH:29][CH:28]=[C:27]([Cl:31])[CH:26]=2)[C:21]([O:23]C)=[O:22])=[CH:17][CH:16]=1)[CH3:2].[OH-].[Na+].Cl>CO>[CH2:1]([C:3]1[N:4]=[C:5]2[C:10]([CH3:11])=[CH:9][C:8]([CH3:12])=[N:7][N:6]2[C:13]=1[CH2:14][C:15]1[CH:16]=[CH:17][C:18]([O:19][CH:20]([C:25]2[CH:30]=[CH:29][CH:28]=[C:27]([Cl:31])[CH:26]=2)[C:21]([OH:23])=[O:22])=[CH:32][CH:33]=1)[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 19784144HCID 19784144, 화합물

생성물 1

HCID 19784136HCID 19784136, 화합물수율 69.1%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a solution of 0.043 g (0.09 mmol) of the product of Step A in 1 mL of methanol was added 0.5 mL of a 1.0N solution of sodium hydroxide and the reaction mixture was stirred at room temperature for 15 hours. The reaction mixture was then adjusted to pH=6 with 0.5 mL of 1.0N hydrochloric acid, then concentrated in vacuo. The residue was purified on a silica gel flash chromatography column eluted with CHCl3 -MeOH-NH4OH (80:15:1). The purified fractions were combined, evaporated and dried in vacuo to afford 0.028 g (67%) of the title compound.

후처리

  1. concentrationconcentrated in vacuo
  2. customThe residue was purified on a silica gel flash chromatography column
  3. washeluted with CHCl3 -MeOH-NH4OH (80:15:1)
  4. customevaporated
  5. customdried in vacuo

출처 및 근거

ORD 기록
ord-583df0511ec442a68b7a23e0097543b0
출처 데이터셋
uspto-grants-1993_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05260285

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