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Hydrochloric Acid → HCID 86633983、化合物

HRID 1687592
ノート
印刷プレビュー

反応式

HRID 1687592 の反応式
[Cl:1][C:2]1[N:7]=[C:6]([NH:8][C:9]2[CH:18]=[C:17]([N+:19]([O-])=O)[CH:16]=[CH:15][C:10]=2[C:11]([NH:13][CH3:14])=[O:12])[C:5]([Cl:22])=[CH:4][N:3]=1.Cl.[OH-].[Na+]>[Fe]>[NH2:19][C:17]1[CH:16]=[CH:15][C:10]([C:11]([NH:13][CH3:14])=[O:12])=[C:9]([NH:8][C:6]2[C:5]([Cl:22])=[CH:4][N:3]=[C:2]([Cl:1])[N:7]=2)[CH:18]=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 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 866339812-(2,5-Dichloro-pyrimidin-4-ylamino)-N-methyl-4-nitro-benzamide

生成物 1

HCID 86633983HCID 86633983、化合物収率 60.1%

試薬・触媒・溶媒 1

HCID 23925Iron触媒

実験手順

2-(2,5-Dichloro-pyrimidin-4-ylamino)-N-methyl-4-nitro-benzamide (0.248 g, 0.72 mmol), Iron (0.202 g, 3.62 mmol), and HCl (3 mL, 0.1 mol) were heated at 50° C. for 1 h. The reaction mixture was neutralized with NaOH and extracted with CH2Cl2. The suspension was filtered, and the resulting solids were washed with CH2Cl2 and EtOAc. The combined organic layers were dried over MgSO4, filtered, and concentrated under reduced pressure to afford 135 mg (60%) title compound.

後処理

  1. extractionextracted with CH2Cl2
  2. filtrationThe suspension was filtered
  3. washthe resulting solids were washed with CH2Cl2 and EtOAc
  4. dry with materialThe combined organic layers were dried over MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-d336194b0107449cb540e16926180442
出典データセット
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08148391B2

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