Hydrazine hydrate (1:1) → HCID 178509389, 화합물

HRID 64256

반응식

HRID 64256 반응식
CO[C:3]([C:9]1[CH:14]=[CH:13][C:12]([O:15][C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)=[CH:11][CH:10]=1)=[C:4]([C:7]#[N:8])[C:5]#[N:6].O.[NH2:23][NH2:24]>C(O)C>[NH2:6][C:5]1[NH:24][N:23]=[C:3]([C:9]2[CH:14]=[CH:13][C:12]([O:15][C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=3)=[CH:11][CH:10]=2)[C:4]=1[C:7]#[N:8]

참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 223472272-((Methoxy)(4-phenoxyphenyl)methylene)malononitrile

생성물 1

HCID 178509389HCID 178509389, 화합물수율 68.8%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a solution of 2-(methoxy(4-phenoxyphenyl)methylene)malononitrile (80 g, 290 mmol) in ethanol (200 mL) was added hydrazine hydrate (20 mL). The mixture was stirred at RT for 16 hr then was concentrated to give the crude product and washed with MeOH (30 mL) to afford 55 g (68.8%) of 5-amino-3-(4-phenoxyphenyl)-1H-pyrazole-4-carbonitrile as a off-white solid. 1H NMR (DMSO-d6) δ 12.11 (br s, 1H), 7.80 (d, J=8.8 Hz, 2H), 7.46-7.39 (m, 2H), 7.18 (t, J=7.6 Hz, 1H), 7.12-7.04 (m, 4H), 6.43 (br s, 2H).

후처리

  1. concentrationthen was concentrated
  2. customto give the crude product
  3. washwashed with MeOH (30 mL)

출처 및 근거

ORD 기록
ord-2b70bc0aa45e45eabbf68769fb969725
출처 데이터셋
uspto-grants-2016_09
특허 번호
US09447106B2

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