3-{5-Cyano-6-[(2,2-dimethyl-propyl)-methyl-amino]-2-methylsulfanyl-pyrimidin-4-ylamino}-N-methoxy-4-methyl-benzamide → 3-{5-Cyano-6-[(2,2-dimethyl-propyl)-methyl-amino]-2-methanesulfinyl-pyrimidin-4-ylamino}-N-methoxy-4-methyl-benzamide

HRID 852032노트

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HRID 852032 반응식
[C:1]([C:3]1[C:4]([NH:18][C:19]2[CH:20]=[C:21]([CH:27]=[CH:28][C:29]=2[CH3:30])[C:22]([NH:24][O:25][CH3:26])=[O:23])=[N:5][C:6]([S:16][CH3:17])=[N:7][C:8]=1[N:9]([CH2:11][C:12]([CH3:15])([CH3:14])[CH3:13])[CH3:10])#[N:2].I([O-])(=O)(=O)=[O:32].[Na+]>C(O)C.O>[C:1]([C:3]1[C:4]([NH:18][C:19]2[CH:20]=[C:21]([CH:27]=[CH:28][C:29]=2[CH3:30])[C:22]([NH:24][O:25][CH3:26])=[O:23])=[N:5][C:6]([S:16]([CH3:17])=[O:32])=[N:7][C:8]=1[N:9]([CH2:11][C:12]([CH3:13])([CH3:14])[CH3:15])[CH3:10])#[N:2]

참가 물질

5

반응물 2

HCID 116976333-{5-Cyano-6-[(2,2-dimethyl-propyl)-methyl-amino]-2-methylsulfanyl-pyrimidin-4-ylamino}-N-methoxy-4-methyl-benzamideHCID 23667635Sodium periodate

생성물 1

HCID 589285033-{5-Cyano-6-[(2,2-dimethyl-propyl)-methyl-amino]-2-methanesulfinyl-pyrimidin-4-ylamino}-N-methoxy-4-methyl-benzamide수율 86.8%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

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온도
70 °C

실험 절차

To a solution of 3-{5-Cyano-6-[(2,2-dimethyl-propyl)-methyl-amino]-2-methylsulfanyl-pyrimidin-4-ylamino}-N-methoxy-4-methyl-benzamide (0.10 g) in ethanol (5 mL) was added the solution of sodium periodate (0.2 g) in water (1 mL). The resulting solution was heated to 70° C. for overnight. The solvent was evaporated and the residue was partitioned between water and ethyl acetate. The organic layer was separated, and concentrated, and the residue was purified by silica gel column chromatography to afford the sulfoxide product (90 mg). MS (m/z): 445 (M+H).

후처리

  1. customThe solvent was evaporated
  2. customthe residue was partitioned between water and ethyl acetate
  3. customThe organic layer was separated
  4. concentrationconcentrated
  5. customthe residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-a12f7a07c0804138907dafb0ff4fb546
출처 데이터셋
uspto-grants-2007_08
특허 번호
US07253174B2

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