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1,4-Dioxane hydrochloride → HCID 117839269、化合物

HRID 1477636
ノート
印刷プレビュー

反応式

HRID 1477636 の反応式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C:10]2[C@@H:15]([O:16][C:17](=[O:22])[C:18]([CH3:21])([CH3:20])[CH3:19])[CH2:14][N:13](C(OC(C)(C)C)=O)[CH2:12][CH:11]=2)=[N:6][C:7]=1[O:8][CH3:9].Cl.O1CCOCC1>CO>[C:17]([O:16][C@@H:15]1[C:10]([C:5]2[CH:4]=[CH:3][C:2]([Cl:1])=[C:7]([O:8][CH3:9])[N:6]=2)=[CH:11][CH2:12][NH:13][CH2:14]1)(=[O:22])[C:18]([CH3:21])([CH3:20])[CH3:19]
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 2

HCID 204431481,4-Dioxane hydrochlorideHCID 117849075HCID 117849075、化合物

生成物 1

HCID 117839269HCID 117839269、化合物収率 127.8%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a methanol solution (1.0 mL) of tert-butyl (R)-5-chloro-6-methoxy-5′-(pivaloyloxy)-5′,6′-dihydro-[2,4′-bipyridine]-1′(2′H)-carboxylate (1.35 g, 3.18 mmol) synthesized in Reference Synthesis Example 142, 4 M hydrogen chloride/1,4-dioxane (15 mL) was added and the resultant mixture was stirred at room temperature for 5 minutes. After completion of the reaction, the reaction solution was concentrated under reduced pressure and saturated sodium bicarbonate aqueous solution and water were added to the concentrated solution, followed by extraction from the resultant mixture with ethyl acetate. The organic layer was concentrated under reduced pressure to obtain a crude product of the title compound (1.32 g).

後処理

  1. additionwas added
  2. customAfter completion of the reaction
  3. concentrationthe reaction solution was concentrated under reduced pressure and saturated sodium bicarbonate aqueous solution and water
  4. additionwere added to the concentrated solution
  5. extractionfollowed by extraction from the resultant mixture with ethyl acetate
  6. concentrationThe organic layer was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-cde83dbd09d34a8fad044e25fbbdf49e
出典データセット
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09403798B2

反応ノート

読み込み中…

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