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Hydrochloric Acid → HCID 58380528、化合物

HRID 1259386
ノート
印刷プレビュー

反応式

HRID 1259386 の反応式
Cl.Cl[Sn]Cl.O.[F:6][C:7]1[CH:12]=[C:11]([I:13])[CH:10]=[CH:9][C:8]=1[NH:14][C:15]1[C:16]([N+:26]([O-])=O)=[C:17]2[O:25][CH2:24][CH2:23][N:18]2[C:19](=[O:22])[C:20]=1[CH3:21].C(=O)(O)[O-]>C(O)C.C(OC(=O)C)C>[NH2:26][C:16]1[C:15]([NH:14][C:8]2[CH:9]=[CH:10][C:11]([I:13])=[CH:12][C:7]=2[F:6])=[C:20]([CH3:21])[C:19](=[O:22])[N:18]2[CH2:23][CH2:24][O:25][C:17]=12
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 4

HCID 313Hydrochloric AcidHCID 769Bicarbonate IonHCID 43835034Tin dichloride dihydrateHCID 583805937-(2-Fluoro-4-iodo-phenylamino)-6-methyl-8-nitro-2,3-dihydro-oxazolo[3,2-a]pyridin-5-one

生成物 1

HCID 58380528HCID 58380528、化合物収率 57.5%

試薬・触媒・溶媒 2

HCID 702
Ethanol
溶媒
HCID 8857Ethyl Acetate溶媒2 回

実験手順

Concentrated HCl (0.2 mL) and SnCl2.H2O (0.24 g, 1.06 mmol) were added to 7-(2-fluoro-4-iodo-phenylamino)-6-methyl-8-nitro-2,3-dihydro-oxazolo[3,2-a]pyridin-5-one (0.15 g, 0.347 mmol) in ethanol (5 mL). The resulting mixture was heated to reflux for 2 hours. The reaction was monitored by TLC (100% ethylacetate). The reaction mixture was cooled to room temperature, diluted with ethylacetate, basified with saturated bicarbonate solution and filtered through celite. The organic layer was washed with brine solution, dried over Na2SO4 and concentrated to afford 0.08 g of the crude product which was used in the next step without further purification.

後処理

  1. temperatureThe resulting mixture was heated
  2. temperatureto reflux for 2 hours
  3. filtrationfiltered through celite
  4. washThe organic layer was washed with brine solution
  5. dry with materialdried over Na2SO4
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-591d17101e174c3aa9559ebfca0581dc
出典データセット
uspto-grants-2013_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08466289B2

反応ノート

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