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Lithium Hydroxide → HCID 58551346, 화합물

HRID 2204254
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HRID 2204254 반응식
[CH2:1]([C:3]1[CH:32]=[CH:31][C:6]([C:7]([N:9]2[CH2:30][CH2:29][C:12]3([C:17]4=[CH:18][CH:19]=[CH:20][N:16]4[C:15]4[CH:21]=[CH:22][C:23]([C:25]([O:27]C)=[O:26])=[CH:24][C:14]=4[O:13]3)[CH2:11][CH2:10]2)=[O:8])=[CH:5][C:4]=1[O:33][CH3:34])[CH3:2].[Li+].[OH-]>O1CCOCC1.C(OCC)(=O)C>[CH2:1]([C:3]1[CH:32]=[CH:31][C:6]([C:7]([N:9]2[CH2:10][CH2:11][C:12]3([O:13][C:14]4[CH:24]=[C:23]([C:25]([OH:27])=[O:26])[CH:22]=[CH:21][C:15]=4[N:16]4[CH:20]=[CH:19][CH:18]=[C:17]34)[CH2:29][CH2:30]2)=[O:8])=[CH:5][C:4]=1[O:33][CH3:34])[CH3:2]
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참가 물질

5

반응물 2

HCID 3939Lithium HydroxideHCID 58550869HCID 58550869, 화합물

생성물 1

HCID 58551346HCID 58551346, 화합물

시약·촉매·용매 2

HCID 8857Ethyl Acetate용매HCID 312751,4-Dioxane용매

실험 절차

A solution of methyl 1-(4-ethyl-3-methoxy-benzoyl)spiro[piperidine-4,4′-pyrrolo[2,1-c][1,4]benzoxazine]-7′-carboxylate (1.1 g, 2.5 mmol) in LiOH (2.5 mL of 4.0 M, 9.9 mmol) and dioxane (5 mL) was stirred at 50° C. for 1 hour. The reaction was diluted with ethyl acetate and washed with water. The aqueous was acidified with 1N HCl and the product was extracted into ethyl acetate. The organics were dried over sodium sulfate, filtered and evaporated to yield a crude product that was used in the next step without further purification (0.60 g, 53%). ESI-MS m/z calc. 446.5, found 447.5 (M+1)+; Retention time: 1.84 minutes (3 min run).

후처리

  1. washwashed with water
  2. extractionthe product was extracted into ethyl acetate
  3. dry with materialThe organics were dried over sodium sulfate
  4. filtrationfiltered
  5. customevaporated

출처 및 근거

ORD 기록
ord-95bc5e1598004269b0491b5d2aab87f8
출처 데이터셋
uspto-grants-2016_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09365588B2

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