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

HRID 2387748
ノート
印刷プレビュー

反応式

HRID 2387748 の反応式
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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 6344DichloromethaneHCID 7864Chloromethyl Methyl EtherHCID 81531DiisopropylethylamineHCID 178432770HCID 178432770、化合物

生成物 2

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
-40 °C

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-6596d1464a1c458f808f6a3bc5bba5f9
出典データセット
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08268848B2

反応ノート

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