홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Dichloromethane → 5-Iodo-4-(methoxymethoxy)-2,6-dimethylpyrimidine

HRID 2387748
노트
인쇄 미리보기

반응식

HRID 2387748 반응식
C(N(CC)C(C)C)(C)C.ClCCl.[I:13][C:14]1[C:15]([OH:22])=[N:16][C:17]([CH3:21])=[N:18][C:19]=1[CH3:20].[CH3:23][O:24][CH2:25]Cl>O>[I:13][C:14]1[C:15](=[O:22])[N:16]([CH2:23][O:24][CH3:25])[C:17]([CH3:21])=[N:18][C:19]=1[CH3:20].[I:13][C:14]1[C:15]([O:22][CH2:23][O:24][CH3:25])=[N:16][C:17]([CH3:21])=[N:18][C:19]=1[CH3:20]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 6344DichloromethaneHCID 7864Chloromethyl Methyl EtherHCID 81531DiisopropylethylamineHCID 178432770HCID 178432770, 화합물

생성물 2

HCID 672831815-Iodo-4-(methoxymethoxy)-2,6-dimethylpyrimidineHCID 674740695-iodo-3-(methoxymethyl)-2,6-dimethylpyrimidin-4(3H)-one

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
-40 °C

실험 절차

N,N-diisopropylethylamine (13.1 ml) was added to a dichloromethane (100 ml) solution of the compound 326-2 (14.5 g). Chloromethyl methyl ether (4.85 ml) was added to the reaction solution, while the solution was stirred at −40° C. The obtained mixture was stirred at room temperature for 15 hours. Water was added to the reaction solution, and the mixture was extracted with dichloromethane. The obtained organic layer was dried over magnesium sulfate and then concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (n-heptane:ethyl acetate=19:1 to 0:1), so as to obtain the title compound (10.6 g) and 5-iodo-4-(methoxymethoxy)-2,6-dimethylpyrimidine (2.55 g).

후처리

  1. stirringThe obtained mixture was stirred at room temperature for 15 hours
  2. extractionthe mixture was extracted with dichloromethane
  3. dry with materialThe obtained organic layer was dried over magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customThe obtained residue was purified by silica gel column chromatography (n-heptane:ethyl acetate=19:1 to 0:1)

출처 및 근거

ORD 기록
ord-6596d1464a1c458f808f6a3bc5bba5f9
출처 데이터셋
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08268848B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트