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Water → 5-chloro-N-chlorocarbonyl-N-{2-[4-(2-ethoxyethyl)-2-methylphenoxy]ethyl}-6-methyl-4-pyrimidine amine

HRID 1460956
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HRID 1460956 반응식
ClC([O:4][C:5]([Cl:8])(Cl)Cl)=O.[Cl:9][C:10]1[C:11]([NH:17][CH2:18][CH2:19][O:20][C:21]2[CH:26]=[CH:25][C:24]([CH2:27][CH2:28][O:29][CH2:30][CH3:31])=[CH:23][C:22]=2[CH3:32])=[N:12][CH:13]=[N:14][C:15]=1[CH3:16].C(N(CC)CC)C.O>C1(C)C=CC=CC=1>[Cl:9][C:10]1[C:11]([N:17]([C:5]([Cl:8])=[O:4])[CH2:18][CH2:19][O:20][C:21]2[CH:26]=[CH:25][C:24]([CH2:27][CH2:28][O:29][CH2:30][CH3:31])=[CH:23][C:22]=2[CH3:32])=[N:12][CH:13]=[N:14][C:15]=1[CH3:16]
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참가 물질

6

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 10426Diphosgene2회HCID 139099695-Chloro-4-{2-[4-(2-ethoxyethyl)-2-methylphenoxy]ethylamino}-6-methylpyrimidine

생성물 1

HCID 150101975-chloro-N-chlorocarbonyl-N-{2-[4-(2-ethoxyethyl)-2-methylphenoxy]ethyl}-6-methyl-4-pyrimidine amine

시약·촉매·용매 1

HCID 1140
Toluene
용매
2회

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온도
5 °C

실험 절차

An amount 2.0 g of trichloromethyl chloroformate (TCF) was dissolved in 30 ml of toluene and cooled to 5° C. or lower. To the solution was added dropwise a solution of 5.0 g of 5-chloro-N-{2-[4-(2-ethoxyethyl)2-methylphenoxy]ethyl}-6-methyl-4-pyrimidine amine and 1.8 g of triethylamine dissolved in 20 ml of toluene, and after the dropwise addition, the mixture was stirred at room temperature for 3 hours. After completion of the reaction, 20 ml of water was added, and the mixture was stirred at room temperature for one hour to decompose excessive TCF.

후처리

  1. additionafter the dropwise addition
  2. additionwas added
  3. stirringthe mixture was stirred at room temperature for one hour

출처 및 근거

ORD 기록
ord-b466e75864cb470e90716710c97d6197
출처 데이터셋
uspto-grants-1991_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05073558

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