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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
ノート
印刷プレビュー

反応式

HRID 350738 の反応式
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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 1

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 23994Zinc触媒HCID 176Acetic Acid溶媒

反応条件

温度
90 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-f5dcf191f3644769b93e18c65b67f4ba
出典データセット
uspto-grants-2007_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07183276B2

反応ノート

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