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Potassium Hydroxide → 2-(N-Ethoxycarbonyl-N-propargylaminomethyl)-pyrimidine

HRID 1491652
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반응식

HRID 1491652 반응식
[CH2:1]([NH:4][C:5](=[O:9])[O:6][CH2:7][CH3:8])[C:2]#[CH:3].[OH-].[K+].Cl[CH2:13][C:14]1[N:19]=[CH:18][CH:17]=[CH:16][N:15]=1>[Cl-].C([N+](CC)(CC)CC1C=CC=CC=1)C.C1(C)C=CC=CC=1>[CH2:7]([O:6][C:5]([N:4]([CH2:13][C:14]1[N:19]=[CH:18][CH:17]=[CH:16][N:15]=1)[CH2:1][C:2]#[CH:3])=[O:9])[CH3:8]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 14797Potassium HydroxideHCID 12155513Ethyl N-propargylcarbamateHCID 128773712-(Chloromethyl)pyrimidine

생성물 1

HCID 189536422-(N-Ethoxycarbonyl-N-propargylaminomethyl)-pyrimidine

시약·촉매·용매 2

HCID 66133Benzyl triethylammonium chloride촉매HCID 1140Toluene
용매

실험 절차

11.5 g (91 mmol) of ethyl N-propargylcarbamate are introduced into 90 ml of toluene, 20.3 g of KOH powder and 0.5 g of triethylbenzylammonium chloride are added, and 13.5 g (104 mmol) of 2-chloromethyl-pyrimidine (German Offenlegungsschrift 2,932,643) are added dropwise at room temperature. The mixture is stirred overnight at room temperature, the salts are filtered off with suction, the filtrate is washed using saturated sodium chloride solution, dried over magnesium sulphate and concentrated, and the concentrate is distilled.

후처리

  1. additionare added
  2. filtrationthe salts are filtered off with suction
  3. washthe filtrate is washed
  4. dry with materialdried over magnesium sulphate
  5. concentrationconcentrated
  6. distillationthe concentrate is distilled

출처 및 근거

ORD 기록
ord-f56dcc419042420997d49f8792098b97
출처 데이터셋
uspto-grants-1994_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05371090

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