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Potassium Carbonate → HCID 67074144, 화합물

HRID 2093750
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HRID 2093750 반응식
[OH:1][C:2]1[CH:33]=[CH:32][C:5]([CH2:6][NH:7][C:8]2[N:13]=[C:12]([O:14][CH2:15][C:16]([F:19])([F:18])[F:17])[N:11]=[C:10]([NH:20][C:21]3[CH:31]=[CH:30][C:24]([C:25]([O:27][CH2:28][CH3:29])=[O:26])=[CH:23][CH:22]=3)[N:9]=2)=[CH:4][CH:3]=1.Br[CH2:35][CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][NH:41][C:42](=[O:48])[O:43][C:44]([CH3:47])([CH3:46])[CH3:45].C([O-])([O-])=O.[K+].[K+]>CN(C=O)C.CCOC(C)=O>[C:44]([O:43][C:42]([NH:41][CH2:40][CH2:39][CH2:38][CH2:37][CH2:36][CH2:35][O:1][C:2]1[CH:33]=[CH:32][C:5]([CH2:6][NH:7][C:8]2[N:13]=[C:12]([O:14][CH2:15][C:16]([F:19])([F:18])[F:17])[N:11]=[C:10]([NH:20][C:21]3[CH:31]=[CH:30][C:24]([C:25]([O:27][CH2:28][CH3:29])=[O:26])=[CH:23][CH:22]=3)[N:9]=2)=[CH:4][CH:3]=1)=[O:48])([CH3:47])([CH3:46])[CH3:45]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 11430Potassium CarbonateHCID 16211353tert-Butyl (6-bromohexyl)carbamateHCID 58223053HCID 58223053, 화합물

생성물 1

HCID 67074144HCID 67074144, 화합물수율 55.9%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857
Ethyl Acetate
용매

반응 조건

온도
65 °C

실험 절차

To a solution of ethyl 4-(4-(4-hydroxybenzylamino)-6-(2,2,2-trifluoroethoxy)-1,3,5-triazin-2-ylamino)benzoate (1.5 g) in DMF (8 mL) was added tert-butyl 6-bromohexylcarbamate (1.1 g) and K2CO3 (0.9 g). The mixture was heated to 65° C. for 16 hours. After cooling to room temperature, the mixture was diluted with EtOAc (250 mL) and washed with water (50 mL) and brine (50 mL). The organic layer was dried over MgSO4 and concentrated. The residue was purified by recrystallization in MeOH to give ethyl 4-(4-(4-(6-(tert-butoxycarbonylamino)hexyloxy)benzylamino)-6-(2,2,2-trifluoroethoxy)-1,3,5-triazin-2-ylamino)benzoate (1.2 g).

후처리

  1. temperatureAfter cooling to room temperature
  2. washwashed with water (50 mL) and brine (50 mL)
  3. dry with materialThe organic layer was dried over MgSO4
  4. concentrationconcentrated
  5. customThe residue was purified by recrystallization in MeOH

출처 및 근거

ORD 기록
ord-09ac06c9eaf64f04acf31f72a8b89191
출처 데이터셋
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08445490B2

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