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Methyl iodide → HCID 58550842, 화합물

HRID 2204256
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HRID 2204256 반응식
[CH3:1]I.[CH2:3]([C:5]1[CH:10]=[CH:9][C:8]([C:11]([N:13]2[CH2:32][CH2:31][C:16]3([C:21]4=[CH:22][CH:23]=[CH:24][N:20]4[C:19]4[CH:25]=[CH:26][C:27]([CH2:29][OH:30])=[CH:28][C:18]=4[O:17]3)[CH2:15][CH2:14]2)=[O:12])=[CH:7][C:6]=1[O:33][CH3:34])[CH3:4].[H-].[Na+]>CN(C=O)C>[CH2:3]([C:5]1[CH:10]=[CH:9][C:8]([C:11]([N:13]2[CH2:14][CH2:15][C:16]3([O:17][C:18]4[CH:28]=[C:27]([CH2:29][O:30][CH3:1])[CH:26]=[CH:25][C:19]=4[N:20]4[CH:24]=[CH:23][CH:22]=[C:21]34)[CH2:31][CH2:32]2)=[O:12])=[CH:7][C:6]=1[O:33][CH3:34])[CH3:4]
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참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 58551320HCID 58551320, 화합물

생성물 1

HCID 58550842HCID 58550842, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

MeI (7.2 μL, 0.12 mmol) was added to a solution of (4-ethyl-3-methoxy-phenyl)-[7′-(hydroxymethyl)spiro[piperidine-4,4′-pyrrolo[2,1-c][1,4]benzoxazine]-1-yl]methanone (50 mg, 0.12 mmol) and NaH (4.6 mg, 0.12 mmol) in DMF (1 mL) and was stirred at room temperature for 1 hour. The reaction was filtered and purified by reverse phase LC-MS (10-99% CH3CN/H2O). Pure fractions were combined and evaporated to yield (4-ethyl-3-methoxyphenyl)(7-(methoxymethyl)spiro[benzo[b]pyrrolo[1,2-d][1,4]oxazine-4,4′-piperidine]-1′-yl)methanone. ESI-MS m/z calc. 446.5, found 447.5 (M+1)+; Retention time: 2.11 minutes (3 min run).

후처리

  1. filtrationThe reaction was filtered
  2. custompurified by reverse phase LC-MS (10-99% CH3CN/H2O)
  3. customevaporated

출처 및 근거

ORD 기록
ord-c98640e45f0a499d87545cb69c470fd2
출처 데이터셋
uspto-grants-2016_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09365588B2

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