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Dimethylformamide → HCID 58134647、化合物

HRID 444757
ノート
印刷プレビュー

反応式

HRID 444757 の反応式
[F:1][C:2]1[C:3]([F:26])=[C:4]2[O:9][CH2:8][C:7]3([CH2:13][CH2:12][CH2:11][CH2:10]3)[N:6]3[CH:14]=[C:15]([C:23]([OH:25])=[O:24])[C:16](=[O:22])[C:17]([C:18]=1[N+:19]([O-])=O)=[C:5]23.CN(C=O)C>C(O)C.C(O)(=O)C.[Pd]>[NH2:19][C:18]1[C:17]2[C:16](=[O:22])[C:15]([C:23]([OH:25])=[O:24])=[CH:14][N:6]3[C:7]4([CH2:13][CH2:12][CH2:11][CH2:10]4)[CH2:8][O:9][C:4]([C:5]=23)=[C:3]([F:26])[C:2]=1[F:1]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 6228DimethylformamideHCID 581347099',10'-difluoro-8'-nitro-7'-oxospiro[cyclopentane-1,3' (2'H)-[7H]pyrido[1,2,3-de][1,4]benzoxazine]-6'-carboxylic acid

生成物 1

HCID 58134647HCID 58134647、化合物収率 84,748.203%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 18476134Acetic acid ethanol溶媒

実験手順

A solution of 9′,10′-difluoro-8′-nitro-7′-oxospiro[cyclopentane-1,3′ (2′H)-[7H]pyrido[1,2,3-de][1,4]benzoxazine]-6′-carboxylic acid (3.9 g, 0.01 mmol) in ethanol/acetic acid (1:1, v/v, 100 mL) was hydrogenated under atmospheric pressure over 10% Pd/C (390 mg) at 80° C. for 18 h. Then 200 mL of DMF were added and the reaction mixture was heated until it became clear. The catalyst was removed by filtration over Celite, which was washed two times with hot DMF and the combined filtrates were concentrated in vacuo to dryness to yield the title compound (2.85 g, 73%) which was used crude in the next step.

後処理

  1. temperaturethe reaction mixture was heated until it
  2. customThe catalyst was removed by filtration over Celite, which
  3. washwas washed two times with hot DMF
  4. concentrationthe combined filtrates were concentrated in vacuo to dryness

出典と根拠

ORDレコード
ord-23b8173d68e145c89c8183301e18d3a7
出典データセット
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08476261B2

反応ノート

読み込み中…

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