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Water → HCID 10283127, 화합물

HRID 1357301
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HRID 1357301 반응식
C[O:2][C:3](=[O:42])[CH:4]([O:12][C:13]1[CH:22]=[CH:21][C:20]2[C:15](=[CH:16][CH:17]=[C:18]([CH2:23][NH:24][C:25]([C:27]3[O:28][C:29]([O:32][C:33]4[CH:38]=[C:37]([Cl:39])[CH:36]=[C:35]([Cl:40])[CH:34]=4)=[CH:30][CH:31]=3)=[O:26])[CH:19]=2)[C:14]=1[Br:41])[CH2:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1.[OH-].[Na+].O>CO>[Br:41][C:14]1[C:15]2[C:20](=[CH:19][C:18]([CH2:23][NH:24][C:25]([C:27]3[O:28][C:29]([O:32][C:33]4[CH:38]=[C:37]([Cl:39])[CH:36]=[C:35]([Cl:40])[CH:34]=4)=[CH:30][CH:31]=3)=[O:26])=[CH:17][CH:16]=2)[CH:21]=[CH:22][C:13]=1[O:12][CH:4]([CH2:5][C:6]1[CH:7]=[CH:8][CH:9]=[CH:10][CH:11]=1)[C:3]([OH:42])=[O:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 14798Sodium HydroxideHCID 69137736HCID 69137736, 화합물

생성물 1

HCID 10283127HCID 10283127, 화합물수율 27.2%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A mixture of 2-[1-bromo-6-({[5-(3,5-dichloro-phenoxy)-furan-2-carbonyl]-amino}-methyl)-naphthalen-2-yloxy]-3-phenyl-propionic acid methyl ester (0.34 g, 0.508 mmol), prepared in the previous step, 1N NaOH (1.50 mL, 1.5 mmol), 5 mL of water and 50 mL of methanol was stirred under nitrogen at room temperature for 18 h (overnight). The methanol was removed under reduced pressure. The solid that formed was collected by filtration and identified as the sodium salt salt of 2-[1-bromo-6-({[5-(3,5-dichloro-phenoxy)-furan-2-carbonyl]-amino}-methyl)-naphthalen-2-yloxy]-3-phenyl-propionic acid (0.1537 g, 46%). The clear filtrate was acidified with 1N HCl. The solid that precipitated was collected by filtration and dried under reduced pressure to give the title compound (0.0905 g, 27%) as a white solid, mp 86-100° C.

후처리

  1. customThe methanol was removed under reduced pressure
  2. customThe solid that formed
  3. filtrationwas collected by filtration
  4. customThe solid that precipitated
  5. filtrationwas collected by filtration
  6. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-6eb84cf3f2ff4862aeca32868f5605e4
출처 데이터셋
uspto-grants-2003_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06589970B2

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