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llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
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Toluene → HCID 89649425、化合物

HRID 2207653
ノート
印刷プレビュー

反応式

HRID 2207653 の反応式
[CH2:1]([O:3][C:4]1[CH:5]=[CH:6][C:7]([F:23])=[C:8]([C:10]2[CH:15]=[C:14]([CH:16]([CH3:18])[CH3:17])[N:13]=[C:12]([C:19](OC)=[O:20])[CH:11]=2)[CH:9]=1)[CH3:2].CC(C[AlH]CC(C)C)C.C1(C)C=CC=CC=1>C1COCC1>[CH2:1]([O:3][C:4]1[CH:5]=[CH:6][C:7]([F:23])=[C:8]([C:10]2[CH:15]=[C:14]([CH:16]([CH3:17])[CH3:18])[N:13]=[C:12]([CH:19]=[O:20])[CH:11]=2)[CH:9]=1)[CH3:2]
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

5

反応物 3

HCID 1140TolueneHCID 14487Diisobutylaluminum hydrideHCID 89649130HCID 89649130、化合物

生成物 1

HCID 89649425HCID 89649425、化合物収率 87.4%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
-78 °C

実験手順

A solution of methyl 4-(5-ethoxy-2-fluoro-phenyl)-6-isopropyl-pyridine-2-carboxylate (which may be prepared as described in Description 115) (0.72 g, 2.27 mmol) in THF (20 mL) was cooled to −78° C. under nitrogen and was treated dropwise with 1M DIBAL in toluene (4.54 mL, 4.54 mmol) over 10 minutes. The mixture was stirred at −78° C. for 2 hrs. The mixture was quenched with satd. aq. NH4Cl solution (5 ml) and the mixture was allowed to reach room temperature and stirred for 30 mins. Celite was added to the mixture and the mixture was stirred for 10 minutes and then filtered through Celite and concentrated to give 4-(5-ethoxy-2-fluoro-phenyl)-6-isopropyl-pyridine-2-carbaldehyde (D116) (0.57 g);

後処理

  1. customThe mixture was quenched with satd
  2. customto reach room temperature
  3. stirringstirred for 30 mins
  4. additionCelite was added to the mixture
  5. stirringthe mixture was stirred for 10 minutes
  6. filtrationfiltered through Celite
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-4b040b9a37c84d7d8dcbff9529ec0577
出典データセット
uspto-grants-2016_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09376436B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート