Hydrazine hydrate (1:1) → HCID 178509389、化合物

HRID 64256

反応式

HRID 64256 の反応式
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]

参加物

4

反応物 2

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

生成物 1

HCID 178509389HCID 178509389、化合物収率 68.8%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-2b70bc0aa45e45eabbf68769fb969725
出典データセット
uspto-grants-2016_09
特許番号
US09447106B2

関連ノート

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