Lithium Hydroxide → HCID 59416800, 화합물

HRID 1184465

반응식

HRID 1184465 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

HCID 59416800HCID 59416800, 화합물수율 100%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

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)+.

후처리

  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

출처 및 근거

ORD 기록
ord-d70a773b14cd436eb3643879360a0ead
출처 데이터셋
uspto-grants-2014_03
특허 번호
US08669249B2

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