Methanesulfonic Acid → 5-(Diisopropoxymethyl)-2-methylpyrimidine

HRID 512199

反応式

HRID 512199 の反応式
[CH3:1][C:2]1[N:7]=[CH:6][C:5](C=O)=[CH:4][N:3]=1.C(O[CH:14]([O:19][CH:20]([CH3:22])[CH3:21])[O:15][CH:16]([CH3:18])[CH3:17])(C)C.CS(O)(=O)=O.C(=O)([O-])[O-].[K+].[K+]>C(O)(C)C>[CH:20]([O:19][CH:14]([O:15][CH:16]([CH3:17])[CH3:18])[C:5]1[CH:4]=[N:3][C:2]([CH3:1])=[N:7][CH:6]=1)([CH3:21])[CH3:22]

参加物

6

反応物 4

HCID 6395Methanesulfonic AcidHCID 11430Potassium CarbonateHCID 78191Propane, 2,2',2''-[methylidynetris(oxy)]tris-HCID 31609702-Methylpyrimidine-5-carbaldehyde

生成物 1

HCID 867162275-(Diisopropoxymethyl)-2-methylpyrimidine収率 29.1%

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

To a mixture of 2-methylpyrimidine-5-carbaldehyde (1.0 g, 8.2 mmol) and triisopropoxymethane (2.3 g, 12 mmol) in isopropanol (15 ml) was added methanesulfonic acid (0.079 g, 0.053 ml, 0.819 mmol). The reaction was stirred at room temperature for 23 hours. Potassium carbonate (1.132 g, 8.19 mmol) was added and the mixture was filtered and the solution was concentrated in vacuo. The crude mixture was purified by flash chromatography to yield 5-(diisopropoxymethyl)-2-methylpyrimidine (536 mg, 29%)

後処理

  1. filtrationthe mixture was filtered
  2. concentrationthe solution was concentrated in vacuo
  3. customThe crude mixture was purified by flash chromatography

出典と根拠

ORDレコード
ord-4fe02f5b96f2459190c5311e99599d9b
出典データセット
uspto-grants-2015_08
特許番号
US09102591B2

関連ノート

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