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Methyl iodide → HCID 86665015, 화합물

HRID 244379
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HRID 244379 반응식
[CH2:1]([N:8]([CH2:45][C:46]1[CH:51]=[CH:50][CH:49]=[CH:48][CH:47]=1)[CH2:9][CH2:10][N:11]1[C:16]2[CH:17]=[C:18]([C:22]([N:24]([CH:38]([CH3:40])[CH3:39])[C@@H:25]3[CH2:30][CH2:29][CH2:28][N:27]([C:31]([O:33][C:34]([CH3:37])([CH3:36])[CH3:35])=[O:32])[CH2:26]3)=[O:23])[C:19]([CH3:21])=[CH:20][C:15]=2[O:14][C:13]([CH2:42][OH:43])([CH3:41])[C:12]1=[O:44])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[H-].[Na+].[CH3:54]I.[Cl-].[NH4+]>CN(C)C=O.C(OCC)(=O)C>[CH2:1]([N:8]([CH2:45][C:46]1[CH:47]=[CH:48][CH:49]=[CH:50][CH:51]=1)[CH2:9][CH2:10][N:11]1[C:16]2[CH:17]=[C:18]([C:22]([N:24]([CH:38]([CH3:39])[CH3:40])[C@@H:25]3[CH2:30][CH2:29][CH2:28][N:27]([C:31]([O:33][C:34]([CH3:36])([CH3:37])[CH3:35])=[O:32])[CH2:26]3)=[O:23])[C:19]([CH3:21])=[CH:20][C:15]=2[O:14][C:13]([CH2:42][O:43][CH3:54])([CH3:41])[C:12]1=[O:44])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 25517Ammonium ChlorideHCID 86665014HCID 86665014, 화합물

생성물 1

HCID 86665015HCID 86665015, 화합물수율 83.7%

시약·촉매·용매 2

HCID 6228Dimethylformamide
용매
HCID 8857Ethyl Acetate용매

실험 절차

To a solution of the obtained 2-methyl-2-propanyl (3R)-3-[({4-[2-(dibenzylamino)ethyl]-2-(hydroxymethyl)-2,7-dimethyl-3-oxo-3,4-dihydro-2H-1,4-benzoxazin-6-yl}carbonyl)(2-propanyl)amino]-1-piperidine carboxylate (22.5 g) in N,N-dimethylformamide (80 ml) were added sodium hydride (1.6 g) and methyl iodide (5.5 g) under ice-cooling. The mixture was stirred for 30 minutes, and then, cooled to room temperature, and further stirred for 2 hours. To the reaction solution was added a saturated aqueous ammonium chloride solution, and the mixture was ethyl acetate. The organic layer was washed with a saturated aqueous sodium chloride solution, and dried over sodium sulfate. The sodium sulfate was removed by filtration, and the filtrate was concentrated under reduced pressure, followed by purification with silica gel chromatography to give the title compound (19.2 g).

후처리

  1. temperaturecooling
  2. stirringfurther stirred for 2 hours
  3. washThe organic layer was washed with a saturated aqueous sodium chloride solution
  4. dry with materialdried over sodium sulfate
  5. customThe sodium sulfate was removed by filtration
  6. concentrationthe filtrate was concentrated under reduced pressure
  7. customfollowed by purification with silica gel chromatography

출처 및 근거

ORD 기록
ord-db9a4a0f103c4631bfe03b98b5bf4659
출처 데이터셋
uspto-grants-2014_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08658639B2

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