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Hydrochloric Acid → HCID 44608378, 화합물

HRID 1943681
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HRID 1943681 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([C:13]([N:15]2[CH2:20][CH2:19][O:18][C:17]3[CH:21]=[N:22][CH:23]=[CH:24][C:16]2=3)=[O:14])[CH:5]=[C:6]([N+:10]([O-:12])=[O:11])[C:7]=1[O:8]C.[Cl-].[Li+].N1CCNCC1.C(=O)([O-])O.[Na+].Cl>CN(C)C=O>[Cl:1][C:2]1[CH:3]=[C:4]([C:13]([N:15]2[CH2:20][CH2:19][O:18][C:17]3[CH:21]=[N:22][CH:23]=[CH:24][C:16]2=3)=[O:14])[CH:5]=[C:6]([N+:10]([O-:12])=[O:11])[C:7]=1[OH:8]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 5

HCID 313Hydrochloric AcidHCID 4837PiperazineHCID 433294Lithium Chloride2회HCID 516892Sodium BicarbonateHCID 66936726HCID 66936726, 화합물

생성물 1

HCID 44608378HCID 44608378, 화합물수율 103.3%

시약·촉매·용매 1

HCID 6228
Dimethylformamide
용매

실험 절차

In a 25 ml flask, (3-chloro-4-methoxy-5-nitro-phenyl)-(2,3-dihydro-pyrido[3,4-b][1,4]oxazin-1-yl)-methanone (176 mg, 0.441 mmol), lithium chloride (42.7 mg, 1.006 mmol), piperazine (65 mg, 0.755 mmol) and N,N-dimethyl formamide (5 ml) were added and stirred at 1000 for 30 minutes. Lithium chloride (42.7 mg, 1.006 mmol) was further added thereto and then stirred at 1000 for 2 hours. After neutralizing with saturated solution of sodium hydrogen carbonate to pH 8 to 9, the mixture was adjusted to pH 6 again by using 1N hydrochloric acid to form solid. The resulting solid was filtered and recrystallized from methanol and tetrahydrofuran to obtain the target compound 36 as yellow solid (153 mg, 91%).

후처리

  1. stirringstirred at 1000 for 2 hours
  2. customto form solid
  3. filtrationThe resulting solid was filtered
  4. customrecrystallized from methanol and tetrahydrofuran

출처 및 근거

ORD 기록
ord-97f2c3372d5243779ce83136a49e6f5e
출처 데이터셋
uspto-grants-2013_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08394792B2

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