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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 383431
ノート
印刷プレビュー

反応式

HRID 383431 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 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

生成物 1

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

試薬・触媒・溶媒 1

HCID 73012-Methyltetrahydrofuran溶媒

実験手順

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]+.

後処理

  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)

出典と根拠

ORDレコード
ord-779712eac7374981886fc23fcbddc9e6
出典データセット
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08367660B2

反応ノート

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