2-Chloro-5-ethylphenylcyanamide → HCID 178436391、化合物

HRID 1274097ノート

反応式

HRID 1274097 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][CH3:9])=[CH:4][C:3]=1[NH:10][C:11]#[N:12].[S:13]([OH:17])(=[O:16])(=[O:15])[CH3:14].[CH2:18]([C:20]1[CH:21]=[C:22]([CH:24]=[CH:25][CH:26]=1)[NH2:23])[CH3:19]>ClC1C=CC=CC=1>[S:13]([OH:17])(=[O:16])(=[O:15])[CH3:14].[CH2:18]([C:20]1[CH:21]=[C:22]([NH:23][C:11]([NH:10][C:3]2[CH:4]=[C:5]([CH2:8][CH3:9])[CH:6]=[CH:7][C:2]=2[Cl:1])=[NH:12])[CH:24]=[CH:25][CH:26]=1)[CH3:19]

参加物

4

反応物 2

HCID 105593012-Chloro-5-ethylphenylcyanamideHCID 867560113-Ethylaniline mesylate

生成物 1

HCID 178436391HCID 178436391、化合物

試薬・触媒・溶媒 1

HCID 7964Chlorobenzene溶媒

実験手順

A mixture of 2-chloro-5-ethylphenylcyanamide (0.6 g, 3.08 mmol), 3-ethylaniline mesylate (0.64 g, 2.93 mmol), and chlorobenzene (12 mL) were combined in a dry round bottom flask equipped with a water cooled condenser under nitrogen and placed in a preheated oil bath (150-160° C.). The reaction mixture was heated for 3 hours. After cooling, the crude reaction product was purified by crystallization from chlorobenzene/diethylether. The resulting crystals were collected by filtration, washed with diethylether, and dried in a vacuum oven (40° C., 15 hours) to yield the title compound, N-(3-ethylphenyl)-N'-(2-chloro-5-ethylphenyl)guanidine mesylate, as a white solid (1.1 g, 91 % yield).

後処理

  1. customwere combined in a dry round bottom flask
  2. customequipped with a water cooled condenser under nitrogen
  3. customplaced in a preheated oil bath
  4. custom(150-160° C.)
  5. temperatureThe reaction mixture was heated for 3 hours
  6. temperatureAfter cooling
  7. customthe crude reaction product
  8. customwas purified by crystallization from chlorobenzene/diethylether
  9. filtrationThe resulting crystals were collected by filtration
  10. washwashed with diethylether
  11. customdried in a vacuum oven (40° C., 15 hours)

出典と根拠

ORDレコード
ord-1c669ab81e5d442c8abb196a2b508d80
出典データセット
uspto-grants-2000_12
特許番号
US06156741

反応ノート

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