Imidazole → 2-Iodomethyl-4-(1-methylethyl)thiazole

HRID 1609322ノート

反応式

HRID 1609322 の反応式
[CH3:1][CH:2]([C:4]1[N:5]=[C:6]([CH2:9]O)[S:7][CH:8]=1)[CH3:3].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.N1C=CN=C1.[I:35]I>C1(C)C=CC=CC=1>[I:35][CH2:9][C:6]1[S:7][CH:8]=[C:4]([CH:2]([CH3:3])[CH3:1])[N:5]=1

参加物

6

反応物 4

HCID 795ImidazoleHCID 807IodineHCID 11776TriphenylphosphineHCID 10678505(4-Isopropylthiazol-2-yl)methanol

生成物 1

HCID 200843302-Iodomethyl-4-(1-methylethyl)thiazole収率 117.7%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
10 °C

実験手順

A mixture composed of 2.5 g of 4-(1-methylethyl)thiazole methanol, 6.3 g of triphenylphosphine, 2.2 g of imidazole and 100 ml of toluene was warmed until all of the solids dissolved. This solution was cooled to 10° C. and 6.1 g of iodine was added. After 2 hr, the mixture was washed with an excess of sodium thiosulfate solution. The aqueous layer was back extracted with ethyl ether and the combined organic layers were washed with brine and then dried (MgSO4). Removal of the solvents in vacuo yielded 5.0 g of 2-iodomethyl-4-(1-methylethyl)thiazole as an oil.

後処理

  1. temperaturewas warmed until all of the solids
  2. dissolutiondissolved
  3. washthe mixture was washed with an excess of sodium thiosulfate solution
  4. extractionThe aqueous layer was back extracted with ethyl ether
  5. washthe combined organic layers were washed with brine
  6. dry with materialdried (MgSO4)
  7. customRemoval of the solvents in vacuo

出典と根拠

ORDレコード
ord-77bf6b619b9349ba8f10284bff8d6d7e
出典データセット
uspto-grants-1995_03
特許番号
US05399702

反応ノート

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