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2-Chloro-3-[2-methyl-4-(5,6,7,8-tetrahydronaphthalen-2-yl)-5-oxazolyl]propionic acid → 3-[2-Methyl-4-(5,6,7,8-tetrahydronaphthalen-2-yl)-5-oxazolyl]propionic acid

HRID 350738
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HRID 350738 반응식
Cl[CH:2]([CH2:6][C:7]1[O:11][C:10]([CH3:12])=[N:9][C:8]=1[C:13]1[CH:22]=[CH:21][C:20]2[CH2:19][CH2:18][CH2:17][CH2:16][C:15]=2[CH:14]=1)[C:3]([OH:5])=[O:4]>C(O)(=O)C.[Zn]>[CH3:12][C:10]1[O:11][C:7]([CH2:6][CH2:2][C:3]([OH:5])=[O:4])=[C:8]([C:13]2[CH:22]=[CH:21][C:20]3[CH2:19][CH2:18][CH2:17][CH2:16][C:15]=3[CH:14]=2)[N:9]=1
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참가 물질

4

반응물 1

HCID 210884672-Chloro-3-[2-methyl-4-(5,6,7,8-tetrahydronaphthalen-2-yl)-5-oxazolyl]propionic acid

생성물 1

HCID 210885803-[2-Methyl-4-(5,6,7,8-tetrahydronaphthalen-2-yl)-5-oxazolyl]propionic acid수율 79%

시약·촉매·용매 2

HCID 23994Zinc촉매HCID 176Acetic Acid용매

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온도
90 °C

실험 절차

To a solution of 2-chloro-3-[2-methyl-4-(5,6,7,8-tetrahydronaphthalen-2-yl)-5-oxazolyl]propionic acid (3.2 g) in acetic acid (30 mL) was added zinc powder (3.25 g) at 90° C. and the mixture was stirred at 90° C. for 15 min. The insoluble material was removed by filtration and the filtrate was concentrated. Water was added to the residue, and the precipitated crystals were collected by filtration and recrystallized from methanol to give 3-[2-methyl-4-(5,6,7,8-tetrahydronaphthalen-2-yl)-5-oxazolyl]propionic acid (2.25 g, yield 79%) as colorless prism crystals. melting point: 135–136° C.

후처리

  1. customThe insoluble material was removed by filtration
  2. concentrationthe filtrate was concentrated
  3. additionWater was added to the residue
  4. filtrationthe precipitated crystals were collected by filtration
  5. customrecrystallized from methanol

출처 및 근거

ORD 기록
ord-f5dcf191f3644769b93e18c65b67f4ba
출처 데이터셋
uspto-grants-2007_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07183276B2

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