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

HRID 2398195
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HRID 2398195 반응식
[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]
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참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-1dd93b45f36845bbbeb3b8dae3e43e40
출처 데이터셋
uspto-grants-1977_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04024183

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