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Pyridine → ethyl 2-(2-bromo-4-cyclopentyl-5-(methoxycarbonyloxy)phenylcarbamoyl)-6-cyano-2H-benzo[b][1,4]oxazine-4(3H)-carboxylate

HRID 1465167
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HRID 1465167 반응식
[C:1]([C:3]1[CH:4]=[CH:5][C:6]2[O:11][CH:10]([C:12]([OH:14])=O)[CH2:9][N:8]([C:15]([O:17][CH2:18][CH3:19])=[O:16])[C:7]=2[CH:20]=1)#[N:2].C(=O)([O-])OC[C:24]1[CH:29]=[C:28]([NH2:30])[C:27]([Br:31])=[CH:26][C:25]=1[CH:32]1[CH2:36][CH2:35][CH2:34][CH2:33]1.N1C=CC=CC=1.C(P1(=O)OP(CCC)(=O)OP(CCC)(=O)[O:49]1)CC.[C:63]([O:66][CH2:67]C)(=[O:65])C>CC1CCCO1>[Br:31][C:27]1[CH:26]=[C:25]([CH:32]2[CH2:33][CH2:34][CH2:35][CH2:36]2)[C:24]([O:65][C:63]([O:66][CH3:67])=[O:49])=[CH:29][C:28]=1[NH:30][C:12]([CH:10]1[O:11][C:6]2[CH:5]=[CH:4][C:3]([C:1]#[N:2])=[CH:20][C:7]=2[N:8]([C:15]([O:17][CH2:18][CH3:19])=[O:16])[CH2:9]1)=[O:14]
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참가 물질

7

반응물 5

HCID 1049PyridineHCID 8857Ethyl AcetateHCID 111923Propylphosphonic anhydrideHCID 593949876-Cyano-4-ethoxycarbonyl-2,3-dihydro-1,4-benzoxazine-2-carboxylic acidHCID 131730194(5-Amino-4-bromo-2-cyclopentyl-phenyl)methyl carbonate

생성물 1

HCID 59394958
ethyl 2-(2-bromo-4-cyclopentyl-5-(methoxycarbonyloxy)phenylcarbamoyl)-6-cyano-2H-benzo[b][1,4]oxazine-4(3H)-carboxylate
수율 99%

시약·촉매·용매 1

HCID 73012-Methyltetrahydrofuran용매

실험 절차

To a solution of 6-cyano-4-ethoxycarbonyl-2,3-dihydro-1,4-benzoxazine-2-carboxylic acid (552 mg, 2.0 mmol) and (5-amino-4-bromo-2-cyclopentyl-phenyl)methyl carbonate (691 mg, 2.20 mmol) in 2-methyltetrahydrofuran (7 mL) at room temperature was added pyridine (404 μL, 5.0 mmol) followed by the addition of T3P (3181 mg, 2.98 mL of 50% w/w solution, 5.0 mmol). The reaction was stirred at room temperature for 1 h. The reaction mixture was diluted with ethyl acetate then quenched with a saturated aqueous solution of NaHCO3 (4 mL) and stirred for 15 min. The layers were separated, and the aqueous layer was extracted once more with ethyl acetate. The combined organic extracts were filtered to give a white solid. The remaining filtrate was dried over Na2SO4, filtered and concentrated in vacuo to obtain a creamy solid. The combined solids were triturated with hexane (5×5 mL) and washed with ethyl acetate (1 mL) and dichloromethane (1 mL) to provide ethyl 2-(2-bromo-4-cyclopentyl-5-(methoxycarbonyloxy)phenylcarbamoyl)-6-cyano-2H-benzo[b][1,4]oxazine-4(3H)-carboxylate as a white solid (403 mg, 99% yield). LC/MS m/z 573.1 [M+H]+.

후처리

  1. customthen quenched with a saturated aqueous solution of NaHCO3 (4 mL)
  2. stirringstirred for 15 min
  3. customThe layers were separated
  4. extractionthe aqueous layer was extracted once more with ethyl acetate
  5. filtrationThe combined organic extracts were filtered
  6. customto give a white solid
  7. dry with materialThe remaining filtrate was dried over Na2SO4
  8. filtrationfiltered
  9. concentrationconcentrated in vacuo
  10. customto obtain a creamy solid
  11. customThe combined solids were triturated with hexane (5×5 mL)
  12. washwashed with ethyl acetate (1 mL) and dichloromethane (1 mL)

출처 및 근거

ORD 기록
ord-5c530812bf9449a2b2a970aec82cb884
출처 데이터셋
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08999976B2

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