Hydrochloric Acid → HCID 86635133、化合物

HRID 1878372ノート

反応式

HRID 1878372 の反応式
[NH:1]([C:3]([C:5]1[N:6]=[CH:7][C:8]([C:11]([O:13][CH2:14][CH3:15])=[O:12])=[N:9][CH:10]=1)=[O:4])[NH2:2].[N:16]([O-])=O.[Na+].O.Cl>ClCCl>[N:1]([C:3]([C:5]1[N:6]=[CH:7][C:8]([C:11]([O:13][CH2:14][CH3:15])=[O:12])=[N:9][CH:10]=1)=[O:4])=[N+:2]=[N-:16]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 23668193Sodium NitriteHCID 66878617HCID 66878617、化合物

生成物 1

HCID 86635133HCID 86635133、化合物収率 95.9%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
5 °C

実験手順

A mixture of ethyl 5-(hydrazinecarbonyl)pyrazine-2-carboxylate (1.00 g, 4.76 mmol), sodium nitrite (1.76 g, 25.5 mmol), water (18 mL) and dichloromethane (18 mL) was cooled to 0to 5° C. (ice-bath) under vigorous stirring. 6M hydrochloric acid (7.4 mL) was added drop-wise over 30 minutes, keeping the temperature under 10° C. After stirring for a further 30 minutes, the organic layer was separated, dried over magnesium sulfate and concentrated under vacuum to afford the title compound (1.01 g).

後処理

  1. customunder 10° C
  2. customthe organic layer was separated
  3. dry with materialdried over magnesium sulfate
  4. concentrationconcentrated under vacuum

出典と根拠

ORDレコード
ord-f15df8baa6f04476903873b785399093
出典データセット
uspto-grants-2012_11
特許番号
US08314091B2

反応ノート

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