홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Lithium Hydroxide → HCID 11305244, 화합물

HRID 2220272
노트
인쇄 미리보기

반응식

HRID 2220272 반응식
Cl.C[O:3][C:4](=[O:8])[CH2:5][CH2:6][NH2:7].[H-].[Na+].Br[CH2:12][C:13]1[CH:14]=[CH:15][C:16]2[O:20][C:19]([C:21]3[CH:26]=[CH:25][C:24]([C:27]4[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=4)=[C:23]([C:33]([F:36])([F:35])[F:34])[CH:22]=3)=[N:18][C:17]=2[CH:37]=1.[Li+].[OH-]>CN(C=O)C.O>[F:35][C:33]([F:34])([F:36])[C:23]1[CH:22]=[C:21]([C:19]2[O:20][C:16]3[CH:15]=[CH:14][C:13]([CH2:12][NH:7][CH2:6][CH2:5][C:4]([OH:3])=[O:8])=[CH:37][C:17]=3[N:18]=2)[CH:26]=[CH:25][C:24]=1[C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 3939Lithium HydroxideHCID 24758Sodium hydrideHCID 2734767Methyl 3-aminopropanoate hydrochlorideHCID 684533265-(Bromomethyl)-2-[2-(trifluoromethyl)[1,1'-biphenyl]-4-yl]-1,3-benzoxazole

생성물 1

HCID 11305244HCID 11305244, 화합물

시약·촉매·용매 2

HCID 962Water
용매
HCID 6228Dimethylformamide용매2회

실험 절차

To a solution of β-alanine methyl ester hydrochloride salt (2 eq) in dry DMF (0.5 M) is added NaH (3.5 eq). After stirring at room temperature for 10 minutes, a solution of 5-bromomethyl-2-(2-trifluoromethyl-biphenyl-4-yl)-benzooxazole (1 eq) in dry DMF (1 M) is added. The resulting mixture is stirred at room temperature for 2 hours. It is diluted with H2O and extracted with EtOAc. The organic solution is washed with brine and dried over Na2SO4. After concentration, the residue is dissolve in MeOH (0.2 M) and treated with 2N LiOH solution (3 eq) for 10 hours. The final compound is purified by preparative LCMS to give 3-{[2-(2-trifluoromethyl-biphenyl-4-yl)-benzooxazol-5-ylmethyl]-amino}-propionic acid; 1H NMR (400 MHz, CD3OD) δ 2.74 (t, J=6.7 Hz, 2H), 3.30 (t, J=6.8 Hz, 2H), 4.39 (s, 2H), 7.34 (m, 2H), 7.43 (m, 3H), 7.57 (m, 2H), 7.78 (d, J=8.3 Hz, 1H), 7.94 (s, 1H), 8.43 (d, J =8.0 Hz, 1H), 8.59 (s, 1H). MS: (ES+): 441.3 (M+1)+.

후처리

  1. stirringThe resulting mixture is stirred at room temperature for 2 hours
  2. extractionextracted with EtOAc
  3. washThe organic solution is washed with brine
  4. dry with materialdried over Na2SO4
  5. concentrationAfter concentration
  6. dissolutionthe residue is dissolve in MeOH (0.2 M)
  7. customThe final compound is purified by preparative LCMS

출처 및 근거

ORD 기록
ord-62e577acedb34499b55449bc74118740
출처 데이터셋
uspto-grants-2008_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07417065B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트