Hydrochloric Acid → HCID 24777543、化合物

HRID 2177036ノート

反応式

HRID 2177036 の反応式
[Sn](Cl)Cl.Cl.[CH3:5][O:6][C:7]1[CH:25]=[CH:24][C:10]([O:11][CH2:12][C:13]2[CH:20]=[CH:19][CH:18]=[C:17]([N+:21]([O-])=O)[C:14]=2[C:15]#[N:16])=[CH:9][CH:8]=1.[OH-].[K+]>>[NH2:21][C:17]1[CH:18]=[CH:19][CH:20]=[C:13]([CH2:12][O:11][C:10]2[CH:9]=[CH:8][C:7]([O:6][CH3:5])=[CH:25][CH:24]=2)[C:14]=1[C:15]#[N:16]

参加物

5

反応物 4

HCID 313Hydrochloric AcidHCID 14797Potassium HydroxideHCID 24479Stannous ChlorideHCID 24777539HCID 24777539、化合物

生成物 1

HCID 24777543HCID 24777543、化合物収率 73%

反応条件

温度
15 °C

実験手順

To a cooled (15° C.) and stirred solution of tin (II) chloride (0.37 g, 1.65 mmol) and con. hydrochloric acid (2.0 mL) was added a solution of 2-(4-methoxyphenoxymethyl)-6-nitrobenzonitrile (100.0 mg, 0.35 mmol). The reaction mixture was slowly warmed to room temperature and stirred for 3 hours. The reaction mixture was poured on to crushed-ice and potassium hydroxide solution, stirred, extracted with dichloromethane, filtered and dried. Purification by silica gel chromatography (1% methanol in dichloromethane) yielded 65 mg of 2-amino-6-(4-methoxyphenoxymethyl)benzonitrile.

後処理

  1. temperatureThe reaction mixture was slowly warmed to room temperature
  2. additionThe reaction mixture was poured on
  3. stirringstirred
  4. extractionextracted with dichloromethane
  5. filtrationfiltered
  6. customdried
  7. customPurification by silica gel chromatography (1% methanol in dichloromethane)

出典と根拠

ORDレコード
ord-d3d40d438e024a5e80eb349602a52c13
出典データセット
uspto-grants-2015_06
特許番号
US09067897B2

反応ノート

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