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O-(2,2,2-Trifluoroethyl)hydroxylamine hydrochloride → 6-[(E)-3-[3-[(Z)-C-methyl-N-(2,2,2-trifluoroethoxy)carbonimidoyl]azetidin-1-yl]-3-oxoprop-1-enyl]-3,4-dihydro-1H-1,8-naphthyridin-2-one

HRID 2172111
ノート
印刷プレビュー

反応式

HRID 2172111 の反応式
Cl.[F:2][C:3]([F:8])([F:7])[CH2:4][O:5][NH2:6].[C:9]([CH:12]1[CH2:15][N:14]([C:16](=[O:30])/[CH:17]=[CH:18]/[C:19]2[CH:20]=[C:21]3[C:26](=[N:27][CH:28]=2)[NH:25][C:24](=[O:29])[CH2:23][CH2:22]3)[CH2:13]1)(=O)[CH3:10]>CO>[O:30]=[C:16]([N:14]1[CH2:15][CH:12](/[C:9](=[N:6]\[O:5][CH2:4][C:3]([F:8])([F:7])[F:2])/[CH3:10])[CH2:13]1)/[CH:17]=[CH:18]/[C:19]1[CH:20]=[C:21]2[C:26](=[N:27][CH:28]=1)[NH:25][C:24](=[O:29])[CH2:23][CH2:22]2
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 19853822O-(2,2,2-Trifluoroethyl)hydroxylamine hydrochlorideHCID 67154676(E)-6-(3-(3-acetylazetidin-1-yl)-3-oxoprop-1-enyl)-3,4-dihydro-1,8-naphthyridin-2(1H)-one

生成物 1

HCID 529507506-[(E)-3-[3-[(Z)-C-methyl-N-(2,2,2-trifluoroethoxy)carbonimidoyl]azetidin-1-yl]-3-oxoprop-1-enyl]-3,4-dihydro-1H-1,8-naphthyridin-2-one収率 74.1%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

2,2,2-Trifluoroethoxyamine hydrochloride (37 mg, 0.24 mmol) was added to a solution of (E)-6-(3-(3-acetylazetidin-1-yl)-3-oxoprop-1-enyl)-3,4-dihydro-1,8-naphthyridin-2(1H)-one (50 mg, 0.16 mmol) in methanol (4 mL). The reaction mixture was stirred at room temperature for 3 hours. After concentration to dryness the residue was diluted by addition of dichloromethane (50 mL) and saturated sodium bicarbonate solution (10 mL). The aqueous phase was extracted with dichloromethane (2×40 mL). The combined organic phases were washed with a saturated solution of sodium chloride (1×20 mL), dried over sodium sulfate, filtered and concentrated to dryness. The residue was purified by chromatography on silica gel using ethyl acetate/methanol (95:5) as eluent to obtain the title product as a white solid (47 mg, 50%).

後処理

  1. concentrationAfter concentration to dryness the residue
  2. additionwas diluted by addition of dichloromethane (50 mL) and saturated sodium bicarbonate solution (10 mL)
  3. extractionThe aqueous phase was extracted with dichloromethane (2×40 mL)
  4. washThe combined organic phases were washed with a saturated solution of sodium chloride (1×20 mL)
  5. dry with materialdried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated to dryness
  8. customThe residue was purified by chromatography on silica gel

出典と根拠

ORDレコード
ord-537ce69c4cb8468a82dd55183f686b2e
出典データセット
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09051321B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート