O-Xylene → 3,4-Dichloro-alpha-(2-imidazolin-2-ylaminomethyl)benzyl alcohol

HRID 1658255

反応式

HRID 1658255 の反応式
[NH2:1][CH2:2][CH:3]([OH:12])[C:4]1[CH:9]=[CH:8][C:7]([Cl:10])=[C:6]([Cl:11])[CH:5]=1.C1(C)C(C)=CC=CC=1.N([C:25]1[NH:26][CH2:27][CH2:28][N:29]=1)[N+]([O-])=O>CC(C)=O>[Cl:11][C:6]1[CH:5]=[C:4]([CH:9]=[CH:8][C:7]=1[Cl:10])[CH:3]([OH:12])[CH2:2][NH:1][C:25]1[NH:29][CH2:28][CH2:27][N:26]=1

参加物

5

反応物 3

HCID 7237O-XyleneHCID 19349alpha-(Aminomethyl)-3,4-dichlorobenzenemethanolHCID 4100422-Nitroamino-2-imidazoline

生成物 1

HCID 540921273,4-Dichloro-alpha-(2-imidazolin-2-ylaminomethyl)benzyl alcohol

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

反応条件

温度
160 °C

実験手順

To a stirred solution of 8 parts of α(aminomethyl)-3,4-dichlorobenzyl alcohol in 4.5 parts of xylene are added 5.2 parts of 2-(nitramino)-2-imidazoline. The whole is heated in an oil-bath at a temperature of about 160°C. till a clear melt is obtained (about 15 minutes). After cooling to about 60°C., the melt is dissolved in acetone and allowed to crystallize. The precipitated product is filtered off and recrystallized from 20 parts of 4-methyl-2-pentanone, yielding 3,4-dichloro-α-(2-imidazolin 2-ylaminomethyl)benzyl alcohol; m.p. 148°C.

後処理

  1. customis obtained (about 15 minutes)
  2. temperatureAfter cooling to about 60°C.
  3. customto crystallize
  4. filtrationThe precipitated product is filtered off
  5. customrecrystallized from 20 parts of 4-methyl-2-pentanone

出典と根拠

ORDレコード
ord-b19a149a41614f8a94dd57c29f724c9f
出典データセット
uspto-grants-1976_06
特許番号
US03963718

関連ノート

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