Methyl iodide → HCID 178512035, 화합물

HRID 499799노트

반응식

HRID 499799 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:17]#[C:18][NH2:19].O.NN>CC#N>[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:19]\[C:18]#[N:17])=[CH:4][CH:3]=1

참가 물질

6

반응물 4

HCID 6328Methyl iodideHCID 9864CyanamideHCID 24654Hydrazine hydrate (1:1)HCID 86616333HCID 86616333, 화합물

생성물 1

HCID 178512035HCID 178512035, 화합물수율 13.5%

시약·촉매·용매 1

HCID 6342Acetonitrile용매2회

실험 절차

To a solution of 1-(4-iodophenyl)pyridine-2(1H)-thione (180 mg, 0.575 mmol) in CH3CN (15 mL), CH3I (0.50 mL, 8.0 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 CH3CN (5 mL). To the solution, cyanamide (200 mg, 4.76 mmol) and hydrazine monohydrate (0.100 mL, 2.06 mmol) were added. After being stirred at room temperature for 2 h, the mixture was purified by HPLC to give (E)-(1-(4-iodophenyl)pyridin-2(1H)-ylidene)cyanamide (25 mg).

후처리

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

출처 및 근거

ORD 기록
ord-78e284f3339045caa9a014e899353d75
출처 데이터셋
uspto-grants-2010_08
특허 번호
US07767697B2

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