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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Triethylamine → 2-(6,7-dichloro-3-oxo-2,3-dihydro-4H-1,4-benzoxazin-4-yl)-N-methyl-N-[(1R)-1-[3'-(methyloxy)-4-biphenylyl]-2-(4-morpholinyl)ethyl]acetamide

HRID 2114419
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HRID 2114419 반응식
[CH3:1][NH:2][C@H:3]([C:11]1[CH:16]=[CH:15][C:14]([C:17]2[CH:22]=[CH:21][CH:20]=[C:19]([O:23][CH3:24])[CH:18]=2)=[CH:13][CH:12]=1)[CH2:4][N:5]1[CH2:10][CH2:9][O:8][CH2:7][CH2:6]1.[Cl:25][C:26]1[C:27]([Cl:41])=[CH:28][C:29]2[O:34][CH2:33][C:32](=[O:35])[N:31]([CH2:36][C:37]([OH:39])=O)[C:30]=2[CH:40]=1.C(N(CC)CC)C.F[P-](F)(F)(F)(F)F.N1(O[P+](N(C)C)(N(C)C)N(C)C)C2C=CC=CC=2N=N1>CN(C=O)C>[Cl:25][C:26]1[C:27]([Cl:41])=[CH:28][C:29]2[O:34][CH2:33][C:32](=[O:35])[N:31]([CH2:36][C:37]([N:2]([CH3:1])[C@H:3]([C:11]3[CH:12]=[CH:13][C:14]([C:17]4[CH:22]=[CH:21][CH:20]=[C:19]([O:23][CH3:24])[CH:18]=4)=[CH:15][CH:16]=3)[CH2:4][N:5]3[CH2:10][CH2:9][O:8][CH2:7][CH2:6]3)=[O:39])[C:30]=2[CH:40]=1
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HCID 8471TriethylamineHCID 151348Benzotriazol-1-yloxy-tris(dimethylamino)phosphonium hexafluorophosphateHCID 574888462-(6,7-Dichloro-3-oxo-2H-benzo[b][1,4]oxazin-4(3H)-yl)acetic acidHCID 57488867(1R)-N-Methyl-1-[3'-(methyloxy)-4-biphenylyl]-2-(4-morpholinyl)ethanamine

생성물 1

HCID 57488866
2-(6,7-dichloro-3-oxo-2,3-dihydro-4H-1,4-benzoxazin-4-yl)-N-methyl-N-[(1R)-1-[3'-(methyloxy)-4-biphenylyl]-2-(4-morpholinyl)ethyl]acetamide
수율 46.2%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

(1R)-N-Methyl-1-[3′-(methyloxy)-4-biphenylyl]-2-(4-morpholinyl)ethanamine (3.3 g, 10 mmol) was dissolved in 100 mL of DMF at room temperature with magnetic stirring. The resulting solution was treated with (6,7-dichloro-3-oxo-2,3-dihydro-4H-1,4-benzoxazin-4-yl)acetic acid (4.3 g, 12 mmol, with 23 wt % LiCl) followed by triethylamine (2.8 mL, 20 mmol) and BOP (5.3 g, 12 mmol). The reaction mixture was maintained at room temperature for 16 h. The reaction mixture was filtered and the filtrate was added slowly to of H2O (300 mL) with vigorous stirring. The precipitate which formed was collected by filtration and further purified by silica gel chromatography (120 g Redisep column, silica, 40 um, 60 Å, 80 mL/min, A: MeOH (with 10% NEt3), B: CH2Cl2, A: 1% for 20 min, 2% for 20 min, 5% for 10 min; detection at 254 nm). The combined fractions were concentrated, and the resulting residue was triturated with MeOH. The white solid was collected by filtration to give the title compound (2.7 g, 46%). MS (ES) m/e 585 [M+H]+.

후처리

  1. filtrationThe reaction mixture was filtered
  2. additionthe filtrate was added slowly to of H2O (300 mL) with vigorous stirring
  3. customThe precipitate which formed
  4. filtrationwas collected by filtration
  5. customfurther purified by silica gel chromatography (120 g Redisep column, silica, 40 um, 60 Å, 80 mL/min
  6. wait2% for 20 min
  7. wait5% for 10 min
  8. concentrationThe combined fractions were concentrated
  9. customthe resulting residue was triturated with MeOH
  10. filtrationThe white solid was collected by filtration

출처 및 근거

ORD 기록
ord-735e148a5a9a459bb7ad54c3bb526444
출처 데이터셋
uspto-grants-2008_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07432258B2

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