Lithium Hydroxide → HCID 11805816、化合物

HRID 1761052ノート

反応式

HRID 1761052 の反応式
C(OC([N:8]1[C:17]2[N:16]=[CH:15][C:14](/[CH:18]=[CH:19]/[C:20]([O:22]CC3C=CC=CC=3)=[O:21])=[CH:13][C:12]=2[CH2:11][CH2:10][CH2:9]1)=O)(C)(C)C.[Li+].[OH-]>Cl.O1CCOCC1>[N:16]1[C:17]2[NH:8][CH2:9][CH2:10][CH2:11][C:12]=2[CH:13]=[C:14](/[CH:18]=[CH:19]/[C:20]([OH:22])=[O:21])[CH:15]=1

参加物

5

反応物 2

HCID 3939Lithium HydroxideHCID 10938089HCID 10938089、化合物

生成物 1

HCID 11805816HCID 11805816、化合物収率 29%

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒HCID 312751,4-Dioxane溶媒

実験手順

Benzyl (E)-3-[8-(tert-butoxycarbonyl)-5,6,7,8-tetrahydro1,8-naphthyridin-3-yl]acrylate (1.21 g, 3.07 mmole) was dissolved in 4 N HCl in dioxane (15 mL). After 18 hr the mixture was concentrated. The residue was taken up in 1:1 MeOH/H2O (15 mL). 1.0 N LiOH (15 mL, 15 mmole) was added and the mixture heated to reflux. After 18 hr the mixture was cooled to RT and concentrated to approximately ⅓ volume. The mixture was adjusted to pH 6 using 10% HCl. The solid was collected by filtration, washed with H2O, and dried in vacuo to give the title compound (180 mg, 29% over 2 steps): MS (ES) m/e 205 (M+H)+.

後処理

  1. concentrationAfter 18 hr the mixture was concentrated
  2. temperaturethe mixture heated to reflux
  3. concentrationconcentrated to approximately ⅓ volume
  4. filtrationThe solid was collected by filtration
  5. washwashed with H2O
  6. customdried in vacuo

出典と根拠

ORDレコード
ord-38b3dbe955fc4e1d89cf90d80bd77171
出典データセット
uspto-grants-2005_01
特許番号
US06846819B1

反応ノート

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