4-Aminobenzyl alcohol → (4-(4-Chloro-5-(trifluoromethyl)pyrimidin-2-ylamino)phenyl)methanol

HRID 886993노트

반응식

HRID 886993 반응식
[Cl:1][C:2]1[C:7]([C:8]([F:11])([F:10])[F:9])=[CH:6][N:5]=[C:4]([NH:12][C:13]2[CH:18]=[CH:17][C:16]([C@H](NC(=O)OC(C)(C)C)C)=[CH:15][CH:14]=2)[N:3]=1.NC1C=CC([CH2:34][OH:35])=CC=1>>[Cl:1][C:2]1[C:7]([C:8]([F:11])([F:9])[F:10])=[CH:6][N:5]=[C:4]([NH:12][C:13]2[CH:18]=[CH:17][C:16]([CH2:34][OH:35])=[CH:15][CH:14]=2)[N:3]=1

참가 물질

3

반응물 2

HCID 693314-Aminobenzyl alcoholHCID 57584789(R)-tert-butyl 1-(4-(4-chloro-5-(trifluoromethyl)pyrimidin-2-ylamino)phenyl)ethylcarbamate

생성물 1

HCID 57584696(4-(4-Chloro-5-(trifluoromethyl)pyrimidin-2-ylamino)phenyl)methanol

실험 절차

C7 was prepared in a manner similar to that described in for making C3 in Step 3 of Example 1 except that 4-aminobenzyl alcohol (2.4 g, 19 mmol) was used instead of C2. When the reaction was complete the reaction mixture was concentrated and dissolved in EtOA. The resultant solution was washed with water, brine, dried over MgSO4, and concentrated. The resultant tan solid was triterated with ether and a small amount of EtOAc, filtered and concentrated to provide C7 as a tan solid. Yield: 2.98 g, 50%. MS+ 304.1. 1H NMR (500 MHz, d6-DMSO) δ: 10.61 (s, 1H), 8.76 (s, 1H), 7.59 (d, 2H), 7.26 (d, 2H), 5.10 (bs, 1H), 4.43 (s, 2H).

후처리

  1. customC7 was prepared in a manner similar to
  2. concentrationwas concentrated
  3. dissolutiondissolved in EtOA
  4. washThe resultant solution was washed with water, brine
  5. dry with materialdried over MgSO4
  6. concentrationconcentrated
  7. filtrationa small amount of EtOAc, filtered
  8. concentrationconcentrated

출처 및 근거

ORD 기록
ord-a44f01a4ed9e4b48a583f4a865573999
출처 데이터셋
uspto-grants-2012_08
특허 번호
US08247411B2

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