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Hydrazine → HCID 178492932, 화합물

HRID 731843
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HRID 731843 반응식
[F:1][C:2]1[CH:3]=[C:4]([C:10](OC)=[C:11]([C:14]#[N:15])[C:12]#[N:13])[CH:5]=[C:6]([O:8][CH3:9])[CH:7]=1.[NH2:18][NH2:19]>CCO>[NH2:13][C:12]1[NH:19][N:18]=[C:10]([C:4]2[CH:5]=[C:6]([O:8][CH3:9])[CH:7]=[C:2]([F:1])[CH:3]=2)[C:11]=1[C:14]#[N:15]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 9321HydrazineHCID 866170152-((3-Fluoro-5-methoxyphenyl)(methoxy)methylene)malononitrile

생성물 1

HCID 178492932HCID 178492932, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

2-((3-fluoro-5-methoxyphenyl)(methoxy)methylene)malononitrile (BA69, 0.029 mol) stirred in EtOH (20 ml) at room temperature under an argon atmosphere. Hydrazine (1.4 ml, 29 mmol) was added and reaction was left stirring for 90 minutes. Reaction mixture was concentrated in vacuo and dried on vacuum pump overnight to yield intermediate 5-amino-3-(3-fluoro-5-methoxyphenyl)-1H-pyrazole-4-carbonitrile (BA73). Formamide (20 ml) was added and reaction was heated to 180° C. under an argon atmosphere overnight. Reaction was cooled and dH2O was added (40 ml) forcing a white precipitate out of solution. Precipitate was collected and washed with dH2O. Solid was dried and purified by silica gel column chromatography [MeOH—CH2Cl2, 10:90] to yield 3-(3-fluoro-5-methoxyphenyl)-1H-pyrazolo[3,4-d]pyrimidin-4-amine (BA75).

후처리

  1. customreaction
  2. waitwas left
  3. customReaction mixture
  4. concentrationwas concentrated in vacuo
  5. customdried on vacuum pump overnight

출처 및 근거

ORD 기록
ord-84d44d32d52d482dba5a9c25d1fdd43e
출처 데이터셋
uspto-grants-2009_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07585868B2

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