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HCID 15614949, 화합물 → HCID 3012986, 화합물

HRID 620366
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HRID 620366 반응식
[Br:1][C:2]1[CH:11]=[CH:10][C:9]2[C:4](=[CH:5][CH:6]=[C:7]([O:16][CH3:17])[C:8]=2[C:12]([F:15])([F:14])[F:13])[C:3]=1[C:18]([N:20]([C:29]([O:31][CH2:32][CH3:33])=[O:30])[CH2:21][C:22]([O:24]C(C)(C)C)=[O:23])=[O:19]>C(O)=O.O>[Br:1][C:2]1[CH:11]=[CH:10][C:9]2[C:4](=[CH:5][CH:6]=[C:7]([O:16][CH3:17])[C:8]=2[C:12]([F:15])([F:13])[F:14])[C:3]=1[C:18]([N:20]([C:29]([O:31][CH2:32][CH3:33])=[O:30])[CH2:21][C:22]([OH:24])=[O:23])=[O:19]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 15614949HCID 15614949, 화합물

생성물 1

HCID 3012986HCID 3012986, 화합물수율 53.5%

시약·촉매·용매 2

HCID 284Formic Acid용매HCID 962Water용매

실험 절차

A suspension of N-[[2-bromo-6-methoxy-5-(trifluoromethyl)-1-naphthalenyl]carbonyl]-N-(ethoxycarbonyl)glycine, 1,1-dimethylethyl ester (4.68 g, 8.76 mmol) in formic acid (150 mL) was stirred at room temperature under a dry nitrogen atmosphere. After 15 minutes, dissolution occurred. After 11/4 hours, the reaction was diluted with water (1.2 L). The aqueous phase was extracted with ether (2×300 mL). The extracts were combined, dried with magnesium sulfate, and the ether was removed. The residue was suspended in water (150 mL) and filtered. The solid was washed with water (2×30 mL) and dried. The crude product was recrystallized in chloroform:hexane twice to yield the title compound as white needles (2.24 g, 53%), m.p. 167°-168.5° C.

후처리

  1. dissolutiondissolution
  2. extractionThe aqueous phase was extracted with ether (2×300 mL)
  3. dry with materialdried with magnesium sulfate
  4. customthe ether was removed
  5. filtrationfiltered
  6. washThe solid was washed with water (2×30 mL)
  7. customdried
  8. customThe crude product was recrystallized in chloroform

출처 및 근거

ORD 기록
ord-0abadca07c244391a4cafaffce6ff9ec
출처 데이터셋
uspto-grants-1989_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04820727

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