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Triethylamine → HCID 46941029, 화합물

HRID 2114367
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HRID 2114367 반응식
F[P-](F)(F)(F)(F)F.N1(O[P+](N(C)C)(N(C)C)N(C)C)C2C=CC=CC=2N=N1.[Cl:28][C:29]1[CH:30]=[CH:31][C:32]2[O:36][C:35](=[O:37])[N:34]([CH2:38][C:39]([OH:41])=O)[C:33]=2[CH:42]=1.[C:43]1([C:59]2[CH:64]=[CH:63][CH:62]=[CH:61][CH:60]=2)[CH:48]=[CH:47][C:46]([C:49]([NH:57][CH3:58])([CH3:56])[CH2:50][N:51]2[CH2:55][CH2:54][CH2:53][CH2:52]2)=[CH:45][CH:44]=1.CCN(CC)CC>CN(C=O)C>[C:43]1([C:59]2[CH:60]=[CH:61][CH:62]=[CH:63][CH:64]=2)[CH:48]=[CH:47][C:46]([C:49]([N:57]([CH3:58])[C:39](=[O:41])[CH2:38][N:34]2[C:33]3[CH:42]=[C:29]([Cl:28])[CH:30]=[CH:31][C:32]=3[O:36][C:35]2=[O:37])([CH3:56])[CH2:50][N:51]2[CH2:55][CH2:54][CH2:53][CH2:52]2)=[CH:45][CH:44]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 151348Benzotriazol-1-yloxy-tris(dimethylamino)phosphonium hexafluorophosphateHCID 3921330(5-Chloro-2-oxo-benzooxazol-3-yl)-acetic acidHCID 57425539HCID 57425539, 화합물

생성물 1

HCID 46941029HCID 46941029, 화합물

시약·촉매·용매 1

HCID 6228
Dimethylformamide
용매

실험 절차

BOP (133 mg, 0.30 mmol) was added to a mixture containing (5-chloro-2-oxo-1,3-benzoxazol-3(2H)-yl)acetic acid (68 mg, 0.30 mmol), 2-(4-biphenylyl)-N-methyl-1-(1-pyrrolidinyl)-2-propanamine (74 mg, 0.25 mmol) and Et3N (0.042 ml, 0.30 mmol) in DMF (3 ml) and the resulting mixture was stirred at room temperature for 16 h. The crude reaction mixture was purified by preparative HPLC (Xterra PrepRP 30×100 mm, 45 mL/min, A: acetonitrile B: water, PH10, A: 50 to 90% over 12 min, UV detection at 214 nm) to give 17.5 mg (13.9%) as a white solid. MS(ES) m/e 504.4 [M+H]+

후처리

  1. customThe crude reaction mixture
  2. customwas purified by preparative HPLC (Xterra PrepRP 30×100 mm, 45 mL/min
  3. waitA: acetonitrile B: water, PH10, A: 50 to 90% over 12 min
  4. customUV detection at 214 nm) to give 17.5 mg (13.9%) as a white solid

출처 및 근거

ORD 기록
ord-ff17e4b88b7f407bb0bf94d6c6c725f7
출처 데이터셋
uspto-grants-2008_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07432258B2

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