Methyl iodide → HCID 54225997、化合物

HRID 1277337ノート

反応式

HRID 1277337 の反応式
[S:1]1[CH2:6][CH2:5][CH2:4][S:3][CH:2]1[CH:7]=[O:8].[CH:9]([N-]C(C)C)(C)C.[Li+].C(NC(C)C)(C)C.C([Li])CCC.[CH2:29]([O:31][C:32](=[O:39])[CH:33]=[CH:34][C:35]([F:38])([F:37])[F:36])[CH3:30].CI.[Cl-].[NH4+]>O1CCCC1>[CH2:29]([O:31][C:32](=[O:39])[CH:33]([CH3:9])[CH:34]([C:2]1([CH:7]=[O:8])[S:3][CH2:4][CH2:5][CH2:6][S:1]1)[C:35]([F:37])([F:38])[F:36])[CH3:30]

参加物

9

反応物 7

HCID 6328Methyl iodideHCID 7912DiisopropylamineHCID 25517Ammonium ChlorideHCID 141226Ethyl 4,4,4-trifluorobut-2-enoateHCID 6379761,3-dithiane-2-carboxaldehydeHCID 2724682Lithium diisopropylamideHCID 178418339Butyllithium

生成物 1

HCID 54225997HCID 54225997、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒3 回

反応条件

温度
0 °C

実験手順

A solution of 1.47 g (10 mMole) of 1,3-dithiane-2-carboxaldehyde in 10 ml of tetrahydrofuran is added to lithium diisopropylamide, prepared from diisopropylamine (1.01 g, 10 mMole) and butyllithium (4.8 ml of a 2.1 M solution, 10 mM) in 20 ml of tetrahydrofuran at -70° C. To the solution is added 1.60 g (9.5 mMole) of 3-trifluoromethylacrylic acid ethyl ester in 5 ml of tetrahydrofuran and the reaction mixture is stirredat -70° C. for 30 minutes after which 1.3 g (10 mMole) of methyl iodide is added and the mixture is maintained at 0° C. for 15 hoursthen poured into aqueous ammonium chloride and extracted with ether. The ether solution is dried and evaporated to give the title compound.

後処理

  1. extractionextracted with ether
  2. dry with materialThe ether solution is dried
  3. customevaporated

出典と根拠

ORDレコード
ord-35d56d23766d46369a92ab7f9973ecc1
出典データセット
uspto-grants-1981_07
特許番号
US04277395

反応ノート

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