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Hydrochloric Acid → HCID 178482356, 화합물

HRID 1644558
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HRID 1644558 반응식
[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[C:8]([NH:12][CH3:13])=[N:7][CH2:6][CH:5]2[C:14]1[CH:19]=[CH:18][C:17]([N+:20]([O-])=O)=[CH:16][CH:15]=1.Cl>C(O)(=O)C.[Fe]>[NH2:20][C:17]1[CH:16]=[CH:15][C:14]([CH:5]2[C:4]3[C:9](=[CH:10][CH:11]=[C:2]([Cl:1])[CH:3]=3)[C:8]([NH:12][CH3:13])=[N:7][CH2:6]2)=[CH:19][CH:18]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 1784823576-chloro-N-methyl-4-(4-nitrophenyl)-3,4-dihydroisoquinolin-1-amine

생성물 1

HCID 178482356HCID 178482356, 화합물

시약·촉매·용매 2

HCID 23925Iron촉매HCID 176Acetic Acid용매

실험 절차

135.2 mg of iron powder were added to a solution of 255 mg of 6-chloro-1-methylamino-4-(4-nitrophenyl)-3,4-dihydroisoquinoline in 4.5-5 ml of glacial acetic acid and then 1.8 ml of concentrated hydrochloric acid were added dropwise, and the mixture was boiled under reflux conditions for 2 hours. The solvent was removed by distillation, and the residue was mixed with water and made alkaline with 2N NaOH. This aqueous phase was extracted with ethyl acetate and purified by MPLC chromatography using an MPRC cartridge with a mixture of 10 parts by volume of ethyl acetate, 5 parts by volume of n-heptane, 5 parts by volume of dichloromethane, 5 parts by volume of methanol and 1 part by volume of concentrated aqueous ammonia solution. Amorphous product.

후처리

  1. customThe solvent was removed by distillation
  2. additionthe residue was mixed with water
  3. extractionThis aqueous phase was extracted with ethyl acetate
  4. custompurified by MPLC chromatography
  5. additionwith a mixture of 10 parts by volume of ethyl acetate, 5 parts by volume of n-heptane, 5 parts by volume of dichloromethane, 5 parts by volume of methanol and 1 part by volume of concentrated aqueous ammonia solution

출처 및 근거

ORD 기록
ord-0d613b64bb67411bab97e9af69dc6a53
출처 데이터셋
uspto-grants-2012_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08124621B2

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