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HCID 15614949、化合物 → HCID 3012986、化合物

HRID 620366
ノート
印刷プレビュー

反応式

HRID 620366 の反応式
[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]
参加物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 15614949HCID 15614949、化合物

生成物 1

HCID 3012986HCID 3012986、化合物収率 53.5%

試薬・触媒・溶媒 2

HCID 284Formic Acid溶媒HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-0abadca07c244391a4cafaffce6ff9ec
出典データセット
uspto-grants-1989_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04820727

反応ノート

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