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Triethylamine → 10-[3-(R)-(1-aminocyclopropyl)pyrrolidin-1-yl]-2,3-dihydro-3-(S)-methyl-7-oxo-7H-pyrido[1,2,3-de][1,4]benzoxazine-6-Carboxylic Acid

HRID 600881
ノート
印刷プレビュー

反応式

HRID 600881 の反応式
C(OC([NH:8][C:9]1([C@@H:12]2[CH2:16][CH2:15][NH:14][CH2:13]2)[CH2:11][CH2:10]1)=O)(C)(C)C.C(N(CC)CC)C.F[C:25]1[CH:26]=[CH:27][C:28]2[C:38](=[O:39])[C:37]([C:40]([OH:42])=[O:41])=[CH:36][N:30]3[C@@H:31]([CH3:35])[CH2:32][O:33][C:34]=1[C:29]=23>CS(C)=O>[NH2:8][C:9]1([C@@H:12]2[CH2:16][CH2:15][N:14]([C:25]3[CH:26]=[CH:27][C:28]4[C:38](=[O:39])[C:37]([C:40]([OH:42])=[O:41])=[CH:36][N:30]5[C@@H:31]([CH3:35])[CH2:32][O:33][C:34]=3[C:29]=45)[CH2:13]2)[CH2:10][CH2:11]1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8471TriethylamineHCID 11117758(R)-t-Butyl (1-(pyrrolidin-3-yl)cyclopropyl)carbamateHCID 67271113(S)-10-Fluoro-3-methyl-7-oxo-2,3-dihydro-7h-[1,4]oxazino[2,3,4-ij]quinoline-6-carboxylic acid

生成物 1

HCID 1027044010-[3-(R)-(1-aminocyclopropyl)pyrrolidin-1-yl]-2,3-dihydro-3-(S)-methyl-7-oxo-7H-pyrido[1,2,3-de][1,4]benzoxazine-6-Carboxylic Acid収率 36.5%

試薬・触媒・溶媒 1

HCID 679
Dimethyl Sulfoxide
溶媒

反応条件

温度
100 °C

実験手順

After adding 3-(R)-[1-(tert-butoxycarbonylamino)cyclopropyl]pyrrolidine (252 mg, 1.12 mmol) and triethylamine (0.50 ml) to dried dimethyl sulfoxide (3 ml), 10-fluoro-2,3-dihydro-3-(S)-methyl-7-oxo-7H-pyrido[1,2,3-de][1,4]benzoxazine-6-carboxylic acid (244 mg, 928 μmol) was added thereto and stirred while heating in an oil bath of 100° C. for 18 hours under a nitrogen atmosphere. After concentrating the reaction solution under a reduce pressure, the residue was dissolved in chloroform (100 ml). After washing the organic layer with a 10% aqueous citric acid solution (50 ml) and saturated saline solution (50 ml), the organic layer was dried over anhydrous sodium sulfate. After filtering, the filtrate was concentrated under a reduced pressure, and after adding dropwise concentrated hydrochloric acid (6 ml) to the residue while cooling with ice, it was stirred at room temperature for 30 minutes. After adding 4 ml of water to the reaction solution and washing this acidic aqueous solution with chloroform (10 ml×3), the pH was adjusted to 12.0 with an aqueous sodium hydroxide solution. After adjusting the pH of the basic aqueous solution to 7.4 with 1 mol/l hydrochloric acid, extraction with chloroform (100 ml×3) was performed. After drying over anhydrous sodium sulfate, the solvent was evapolated under a reduced pressure. The residue thus obtained was purified by recrystallization from ethanol and then dried under a reduced pressure. 125 mg (36.5%) of the title compound was thereby obtained in the form of yellow crystals.

後処理

  1. additionwas added
  2. concentrationAfter concentrating the reaction solution under a reduce pressure
  3. dissolutionthe residue was dissolved in chloroform (100 ml)
  4. washAfter washing the organic layer with a 10% aqueous citric acid solution (50 ml) and saturated saline solution (50 ml)
  5. dry with materialthe organic layer was dried over anhydrous sodium sulfate
  6. filtrationAfter filtering
  7. concentrationthe filtrate was concentrated under a reduced pressure
  8. additionafter adding dropwise concentrated hydrochloric acid (6 ml) to the residue
  9. temperaturewhile cooling with ice, it
  10. stirringwas stirred at room temperature for 30 minutes
  11. additionAfter adding 4 ml of water to the reaction solution
  12. washwashing this acidic aqueous solution with chloroform (10 ml×3)
  13. extractionwith 1 mol/l hydrochloric acid, extraction with chloroform (100 ml×3)
  14. dry with materialAfter drying over anhydrous sodium sulfate
  15. customThe residue thus obtained
  16. customwas purified by recrystallization from ethanol
  17. customdried under a reduced pressure

出典と根拠

ORDレコード
ord-339fd78624334dd4b159093cc3bd0cf2
出典データセット
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07902226B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート