Isopropyl Acetate → (6-Chloro-pyridin-3-yl)-(4-cyclobutyl-[1,4]diazepan-1-yl)-methanone

HRID 404547ノート

反応式

HRID 404547 の反応式
[Cl:1][C:2]1[N:7]=[CH:6][C:5]([C:8]([N:10]2[CH2:16][CH2:15][CH2:14][N:13]([CH:17]3[CH2:20][CH2:19][CH2:18]3)[CH2:12][CH2:11]2)=[O:9])=[CH:4][CH:3]=1.C(O)(=O)[C@@H]([C@H](C(O)=O)O)O.C(OC(C)=O)(C)C.[OH-].[Na+]>>[Cl:1][C:2]1[N:7]=[CH:6][C:5]([C:8]([N:10]2[CH2:16][CH2:15][CH2:14][N:13]([CH:17]3[CH2:20][CH2:19][CH2:18]3)[CH2:12][CH2:11]2)=[O:9])=[CH:4][CH:3]=1

参加物

4

反応物 3

HCID 7915Isopropyl AcetateHCID 14798Sodium HydroxideHCID 86661641(6-chloro-pyridin-3-yl)-(4-cyclobutyl-[1,4]diazepan-1-yl)-methanone L-tartaric acid

生成物 1

HCID 58076653(6-Chloro-pyridin-3-yl)-(4-cyclobutyl-[1,4]diazepan-1-yl)-methanone

実験手順

A mixture of (6-chloro-pyridin-3-yl)-(4-cyclobutyl-[1,4]diazepan-1-yl)-methanone-L-tartaric acid (172 g, 386.9 mmol), iPrOAc (1.5 L), and 1 N NaOH(aq) (1.5 L) was thoroughly mixed and the resulting layers were separated. The aqueous layer was extracted with additional iPrOAc (1.5 L) and the combined organic layers were dried over magnesium sulfate. After filtration and concentration, (6-chloro-pyridin-3-yl)-(4-cyclobutyl-[1,4]diazepam-1-yl)-methanone was obtained as a yellow oil.

後処理

  1. additionwas thoroughly mixed
  2. customthe resulting layers were separated
  3. extractionThe aqueous layer was extracted with additional iPrOAc (1.5 L)
  4. dry with materialthe combined organic layers were dried over magnesium sulfate
  5. filtrationAfter filtration and concentration
  6. custom(6-chloro-pyridin-3-yl)-(4-cyclobutyl-[1,4]diazepam-1-yl)-methanone was obtained as a yellow oil

出典と根拠

ORDレコード
ord-f2618380e71d4719ae59d15897339bce
出典データセット
uspto-grants-2014_06
特許番号
US08748596B2

反応ノート

読み込み中…