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Ammonia → 1-(3-Isopropylguanidino)-3-(3-p-chlorophenylureido)benzene hydrochloride

HRID 2398195
ノート
印刷プレビュー

反応式

HRID 2398195 の反応式
[CH:1]([NH:4][C:5](=S)[NH:6][C:7]1[CH:12]=[CH:11][CH:10]=[C:9]([NH:13][C:14]([NH:16][C:17]2[CH:22]=[CH:21][C:20]([Cl:23])=[CH:19][CH:18]=2)=[O:15])[CH:8]=1)([CH3:3])[CH3:2].[NH3:25]>C(O)C>[ClH:23].[CH:1]([NH:4][C:5](=[NH:25])[NH:6][C:7]1[CH:12]=[CH:11][CH:10]=[C:9]([NH:13][C:14]([NH:16][C:17]2[CH:22]=[CH:21][C:20]([Cl:23])=[CH:19][CH:18]=2)=[O:15])[CH:8]=1)([CH3:3])[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 222AmmoniaHCID 538688891-(3-Isopropylthioureido)-3-(3-p-chlorophenylureido)benzene

生成物 1

HCID 1784575781-(3-Isopropylguanidino)-3-(3-p-chlorophenylureido)benzene hydrochloride

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

1-(3-Isopropylthioureido)-3-(3-p-chlorophenylureido)-benzene (1.5 crystallized g.) is dissolved in ethanol (100 ml.) saturated with ammonia gas, and the solution stirred for 24 hours at room temperature with yellow mercuric oxide (1.02 g.). The mixture is boiled for 1/2 hour to coagulate the fine precipitate, and is filtered hot. The solid is washed thoroughly with 3 × 50 ml. portions of boiling ethanol, and the filtrate and washings are combined and evaporated to dryness. The remaining gum is dissolved in methanol (10 ml.) and saturated ethereal hydrogen chloride (3 ml.) is added followed by dry ether (150 ml.). The precipitated oil rapidly solidifies, is filtered off and crystallised from ethanol to give 1-(3-isopropylguanidino)-3-(3-p-chlorophenylureido)benzene hydrochloride, m.p. 224°-225° C.

後処理

  1. filtrationis filtered hot
  2. washThe solid is washed thoroughly with 3 × 50 ml
  3. customevaporated to dryness
  4. dissolutionThe remaining gum is dissolved in methanol (10 ml.)
  5. additionsaturated ethereal hydrogen chloride (3 ml.) is added
  6. filtrationis filtered off
  7. customcrystallised from ethanol

出典と根拠

ORDレコード
ord-1dd93b45f36845bbbeb3b8dae3e43e40
出典データセット
uspto-grants-1977_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04024183

反応ノート

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