2-Methyl-1,3-dithiane → HCID 19862733、化合物

HRID 1721964

反応式

HRID 1721964 の反応式
C([Li])CCC.[CH3:6][CH:7]1[S:12][CH2:11][CH2:10][CH2:9][S:8]1.Br[CH2:14][CH2:15][CH2:16][CH2:17][O:18][CH2:19][CH2:20][CH2:21][C:22]1[CH:27]=[CH:26][C:25]([N:28]2[CH2:32][CH2:31][CH2:30][CH2:29]2)=[CH:24][CH:23]=1>C1COCC1>[CH3:6][C:7]1([CH2:14][CH2:15][CH2:16][CH2:17][O:18][CH2:19][CH2:20][CH2:21][C:22]2[CH:27]=[CH:26][C:25]([N:28]3[CH2:32][CH2:31][CH2:30][CH2:29]3)=[CH:24][CH:23]=2)[S:12][CH2:11][CH2:10][CH2:9][S:8]1

参加物

5

反応物 3

HCID 223292-Methyl-1,3-dithianeHCID 19862698HCID 19862698、化合物HCID 178418339Butyllithium

生成物 1

HCID 19862733HCID 19862733、化合物収率 45.5%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

n-Butyllithium (1.5M in hexane, 12 ml) was added over 5 min to a stirred solution of 2-methyl-1,3-dithiane (2.4 g) in dry THF (30 ml) at 70° under nitrogen. The yellow solution was then stirred at -30° to -20° for 2 h, cooled to -78° and treated with a solution of the product of stage (iii) (6.1 g) in THF (25 ml). The solution was stirred at room temperature overnight, the solvent was evaporated and the residue was purified by FCC (hexane→System D 9:1) to give the title compound as a pale yellow oil (3.2 g) T.l.c. (System D 9:1) Rf 0.18.

後処理

  1. temperaturecooled to -78°
  2. stirringThe solution was stirred at room temperature overnight
  3. customthe solvent was evaporated
  4. customthe residue was purified by FCC (hexane→System D 9:1)

出典と根拠

ORDレコード
ord-6c496853f4524094953f62927c492981
出典データセット
uspto-grants-1989_08
特許番号
US04853381

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