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Dichloromethane → 2-(cis-2-Amino-cyclohexylamino)-thieno[3,2-d]pyrimidine-7-carboxylic acid (2,4-dimethoxy-phenyl)-amide

HRID 1773621
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반응식

HRID 1773621 반응식
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([O:9][CH3:10])[CH:6]=[CH:5][C:4]=1[NH:11][C:12]([C:14]1[C:18]2[N:19]=[C:20](Cl)[N:21]=[CH:22][C:17]=2[S:16][CH:15]=1)=[O:13].[C@@H:24]1([NH2:31])[CH2:29][CH2:28][CH2:27][CH2:26][C@@H:25]1[NH2:30].ClCCl>O1CCOCC1>[CH3:1][O:2][C:3]1[CH:8]=[C:7]([O:9][CH3:10])[CH:6]=[CH:5][C:4]=1[NH:11][C:12]([C:14]1[C:18]2[N:19]=[C:20]([NH:30][C@@H:25]3[CH2:26][CH2:27][CH2:28][CH2:29][C@@H:24]3[NH2:31])[N:21]=[CH:22][C:17]=2[S:16][CH:15]=1)=[O:13]
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참가 물질

5

반응물 3

HCID 6344DichloromethaneHCID 3429171,2-Diaminocyclohexane, cis-HCID 870961102-Chloro-thieno[3,2-d]pyrimidine-7-carboxylic acid(2,4-dimethoxy-phenyl)-amide

생성물 1

HCID 566467652-(cis-2-Amino-cyclohexylamino)-thieno[3,2-d]pyrimidine-7-carboxylic acid (2,4-dimethoxy-phenyl)-amide

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

To a solution of 0.047 g (0.134 mmole) 2-chloro-thieno[3,2-d]pyrimidine-7-carboxylic acid(2,4-dimethoxy-phenyl)-amide in 1.34 mL of dioxane was added 0.0967 mL (0.806 mmole) of (cis-cyclohexane-1,2-diamine. The mixture was heated at 100 degrees for over night. Dichloromethane was added and washed with aqueous sodium bicarbonate. The aqueous layer was washed twice with dichloromethane. The organic layer was washed with brine, dried over anhydrous sodium sulfate, filtered and concentrated under reduced pressure. Purification by silica gel chromatography, eluting with dichloromethane-0.7 N ammonia solution in methanol (gradient 100:0-90:10) gave 0.052 g of 2-(cis-2-amino-cyclohexylamino)-thieno[3,2-d]pyrimidine-7-carboxylic acid (2,4-dimethoxy-phenyl)-amide as a yellow solid. MH+/Z=428

후처리

  1. temperatureThe mixture was heated at 100 degrees for over night
  2. washwashed with aqueous sodium bicarbonate
  3. washThe aqueous layer was washed twice with dichloromethane
  4. washThe organic layer was washed with brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure
  8. customPurification by silica gel chromatography
  9. washeluting with dichloromethane-0.7 N ammonia solution in methanol (gradient 100:0-90:10)

출처 및 근거

ORD 기록
ord-5a3296755c794aaea4cb32a2821db715
출처 데이터셋
uspto-grants-2016_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09255110B2

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