Lithium Hydroxide → HCID 59416800、化合物

HRID 1184465

反応式

HRID 1184465 の反応式
[F:1][C:2]1[CH:7]=[C:6]([C:8]([O:10]C)=[O:9])[CH:5]=[CH:4][C:3]=1[N:12]1[CH2:17][CH2:16][N:15]([C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19])[CH2:14][CH2:13]1.[Li+].[OH-]>O1CCOCC1>[C:21]([O:20][C:18]([N:15]1[CH2:16][CH2:17][N:12]([C:3]2[CH:4]=[CH:5][C:6]([C:8]([OH:10])=[O:9])=[CH:7][C:2]=2[F:1])[CH2:13][CH2:14]1)=[O:19])([CH3:24])([CH3:22])[CH3:23]

参加物

4

反応物 2

HCID 3939Lithium HydroxideHCID 23117202Tert-butyl 4-(2-fluoro-4-(methoxycarbonyl)phenyl)piperazine-1-carboxylate

生成物 1

HCID 59416800HCID 59416800、化合物収率 100%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

tert-butyl 4-(2-fluoro-4-(methoxycarbonyl)phenyl)piperazine-1-carboxylate 301 (4.6 g, 13.59 mmol) was suspended in 1,4-dioxane (68.0 mL) and treated with 1N LiOH (68.0 mL, 68.0 mmol). The reaction mixture was stirred at room temperature for 23 h. The reaction mixture was concentrated in vacuo until most of the dioxane was gone and acidified with HCl (4.5 N) until a thick precipitate resulted. The precipitate was filtered, washed with water, and dried in vacuum to afford the title compound as a brown solid (4.40 g, 13.57 mmol, 100% yield). ESI-MS: m/z 325 (M+H)+.

後処理

  1. concentrationThe reaction mixture was concentrated in vacuo until most of the dioxane
  2. customresulted
  3. filtrationThe precipitate was filtered
  4. washwashed with water
  5. customdried in vacuum

出典と根拠

ORDレコード
ord-d70a773b14cd436eb3643879360a0ead
出典データセット
uspto-grants-2014_03
特許番号
US08669249B2

関連ノート

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