Cyanamide → HCID 178419031, 화합물

HRID 853746

반응식

HRID 853746 반응식
[CH2:1]([O:8][C:9]1[CH:10]=[C:11]([CH:13]=[CH:14][CH:15]=1)[NH2:12])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[N:16]#[C:17][NH2:18]>Cl.O1CCOCC1>[CH2:1]([O:8][C:9]1[CH:10]=[C:11]([NH:12][C:17]([NH2:18])=[NH:16])[CH:13]=[CH:14][CH:15]=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

참가 물질

5

반응물 2

HCID 9864CyanamideHCID 928923-Benzyloxyaniline

생성물 1

HCID 178419031HCID 178419031, 화합물수율 37.3%

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매HCID 312751,4-Dioxane용매

반응 조건

온도
120 °C

실험 절차

3-benzyloxy aniline (1 g, 5 mmol) and cyanamide (420 mg, 10 mmol) were dissolved in 4 mL of 4N HCl in dioxane and heated to 120° C. overnight. The reaction mixture was cooled to room temperature, quenched with water, and extracted with diethyl ether. The aqueous layer was made basic with 2N NaOH and extracted thrice with dichloromethane. The organic extracts were combined and washed with brine, dried over MgSO4, and concentrated to afford 4 (450 mg) as a light brown solid.

후처리

  1. temperatureThe reaction mixture was cooled to room temperature
  2. customquenched with water
  3. extractionextracted with diethyl ether
  4. extractionextracted thrice with dichloromethane
  5. washwashed with brine
  6. dry with materialdried over MgSO4
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-9c1441823c7045499d65031e470e6ed1
출처 데이터셋
uspto-grants-2007_08
특허 번호
US07256190B2

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