Ammonia → HCID 178474184, 화합물

HRID 2357816노트

반응식

HRID 2357816 반응식
[I:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[CH:13]=[CH:12][CH:11]=[CH:10][C:9]2=S)=[CH:4][CH:3]=1.CI.N.CO.[CH2:20]([N:22](CC)CC)[CH3:21].C(Cl)(=[O:29])C>CC#N.CN(C=O)C.N1C=CC=CC=1.C(Cl)Cl>[I:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[CH:13]=[CH:12][CH:11]=[CH:10]/[C:9]/2=[N:22]\[C:20](=[O:29])[CH3:21])=[CH:4][CH:3]=1

참가 물질

11

반응물 6

HCID 222AmmoniaHCID 887MethanolHCID 6328Methyl iodideHCID 6367Acetyl chlorideHCID 8471TriethylamineHCID 86616333HCID 86616333, 화합물

생성물 1

HCID 178474184HCID 178474184, 화합물수율 28.9%

시약·촉매·용매 4

HCID 1049Pyridine용매HCID 6228Dimethylformamide용매HCID 6342Acetonitrile용매HCID 6344Dichloromethane용매

실험 절차

To a solution of 1-(4-iodophenyl)pyridine-2(1H)-thione (384 mg, 1.23 mmol) in CH3CN (10 mL), CH3I (0.80 mL, 12.8 mmol) was added. After being stirred at room temperature overnight, the mixture was concentrated in vacuo to give a solid. The solid was dissolved in DMF (6 mL). To the solution, NH3 in MeOH (7N, 3.0 mL, 21.0 mmol) and triethylamine (1.5 mL, 10.8 mmol) were added. After being stirred at room temperature overnight, the mixture was purified by HPLC to give a solid. The solid was dissolved in pyridine (3 mL) and CH2Cl2 (3 mL). To the solution, acetyl chloride (0.200 mL, 2.8 mmol) was added. After being stirred at room temperature overnight, the mixture was purified by HPLC to give (E)-N-(1-(4-iodophenyl)pyridin-2(1H)-ylidene)acetamide (120 mg).

후처리

  1. concentrationthe mixture was concentrated in vacuo
  2. customto give a solid
  3. stirringAfter being stirred at room temperature overnight
  4. customthe mixture was purified by HPLC
  5. customto give a solid
  6. stirringAfter being stirred at room temperature overnight
  7. customthe mixture was purified by HPLC

출처 및 근거

ORD 기록
ord-d0aaabb21c944ada8b0110715410dec8
출처 데이터셋
uspto-grants-2010_07
특허 번호
US07763608B2

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