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Hydrochloric Acid → HCID 86633983, 화합물

HRID 1687592
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HRID 1687592 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

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

생성물 1

HCID 86633983HCID 86633983, 화합물수율 60.1%

시약·촉매·용매 1

HCID 23925Iron촉매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d336194b0107449cb540e16926180442
출처 데이터셋
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08148391B2

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