2-Methyl-1,3-dithiane → HCID 19862733, 화합물

HRID 1721964

반응식

HRID 1721964 반응식
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

참가 물질

5

반응물 3

HCID 223292-Methyl-1,3-dithianeHCID 19862698HCID 19862698, 화합물HCID 178418339Butyllithium

생성물 1

HCID 19862733HCID 19862733, 화합물수율 45.5%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-6c496853f4524094953f62927c492981
출처 데이터셋
uspto-grants-1989_08
특허 번호
US04853381

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