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3-Bromobenzyl alcohol → 2-(3-Bromobenzyloxy)-5-fluoropyrimidin-4-ylamine

HRID 705558
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HRID 705558 반응식
CC([O-])(C)C.[K+].[Br:7][C:8]1[CH:9]=[C:10]([CH2:14][OH:15])[CH:11]=[CH:12][CH:13]=1.Cl[C:17]1[N:22]=[C:21]([NH2:23])[C:20]([F:24])=[CH:19][N:18]=1>O>[Br:7][C:8]1[CH:9]=[C:10]([CH:11]=[CH:12][CH:13]=1)[CH2:14][O:15][C:17]1[N:22]=[C:21]([NH2:23])[C:20]([F:24])=[CH:19][N:18]=1
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참가 물질

5

반응물 3

HCID 851413-Bromobenzyl alcoholHCID 2543722-Chloro-5-fluoropyrimidin-4-amineHCID 23665647Potassium tert-butoxide

생성물 1

HCID 578188342-(3-Bromobenzyloxy)-5-fluoropyrimidin-4-ylamine수율 49.3%

시약·촉매·용매 1

HCID 962Water용매

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온도
90 °C

실험 절차

To a magnetically stirred mixture of KOtBu (1.0 M in tBuOH, 1.36 ml, 1.36 mmol) was added (3-bromophenyl)methanol (0.25 g, 1.36 mmol). To the resulting solution was added 2-chloro-5-fluoropyrimidine-4-ylamine (0.10 g, 0.68 mmol) and the mixture was capped and stirred at 90° C. for 4 h. The reaction mixture was cooled to room temperature, diluted with water, and the resulting precipitate was collected by filtration. The solid was washed with water, washed with cyclohexane, and dried in the vacuum oven. A CH2Cl2 solution of the compound was loaded onto Biotage SCX column and eluted with CH2Cl2 followed by 2.0 M NH3 in MeOH. The solvent was evaporated under reduced pressure to give the title compound (0.100 g, 49%) as an off-white solid: mp 143-145° C.; 1H NMR (400 MHz, DMSO-d6) δ 7.90 (d, J=2.5 Hz, 1H), 7.61 (s, 1H), 7.43 (d, J=8.0 Hz, 1H), 7.36 (d, J=7.7 Hz, 1H), 7.22 (t, J=7.7 Hz, 1H), 5.28 (s, 2H), 5.20 (br s, 2H); GCMS (EI) m/z 297, 299 (M)+.

후처리

  1. customthe mixture was capped
  2. temperatureThe reaction mixture was cooled to room temperature
  3. filtrationthe resulting precipitate was collected by filtration
  4. washThe solid was washed with water
  5. washwashed with cyclohexane
  6. customdried in the vacuum oven
  7. washeluted with CH2Cl2
  8. customThe solvent was evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-974a0a9392874bb184fb5a37f029953f
출처 데이터셋
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09174970B2

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