Water → HCID 20386919, 화합물

HRID 866368노트

반응식

HRID 866368 반응식
S1CCS[CH:2]1[CH2:6][CH2:7][CH:8]1[CH:19](/[CH:20]=[CH:21]/[CH:22]([OH:28])[CH2:23][CH2:24][CH2:25][CH2:26][CH3:27])[CH2:18][CH2:17][C:9]21[O:14][CH2:13][C:12]([CH3:16])([CH3:15])[CH2:11][O:10]2.[O:29]1[CH2:34][CH2:33][CH2:32][CH2:31][CH:30]1OC1CCCCO1.CI.C([O-])([O-])=[O:45].[Ca+2].O>CN(C=O)C.CC(C)=O>[CH3:15][C:12]1([CH3:16])[CH2:11][O:10][C:9]2([CH2:17][CH2:18][CH:19](/[CH:20]=[CH:21]/[CH:22]([CH2:23][CH2:24][CH2:25][CH2:26][CH3:27])[O:28][CH:30]3[CH2:31][CH2:32][CH2:33][CH2:34][O:29]3)[CH:8]2[CH2:7][CH2:6][CH:2]=[O:45])[O:14][CH2:13]1

참가 물질

7

반응물 4

HCID 962WaterHCID 6328Methyl iodideHCID 10112Calcium CarbonateHCID 86735829HCID 86735829, 화합물

생성물 1

HCID 20386919HCID 20386919, 화합물

시약·촉매·용매 2

HCID 180Acetone용매HCID 6228Dimethylformamide용매

실험 절차

1.05 g (2.05 mmoles of 1-[7-[(1,3-dithia-2-cyclopentyl)ethyl]3,3-dimethyl-1,5-dioxaspiro[5,4]-dec-8-yl]-trans-1-octene-3-ol-tetrahydropyranyl ether was stirred for 2 hours at 50° C in 100 ml of DMF with 0.7 ml (10.3 mmoles) of methyl iodide, 1.4 g (14 moles) of CaCO3 and 0.4 ml of H2O. The solution was cooled, combined with 50 ml of acetone, filtered with suction to remove the precipitate and the filtrate was evaporated to dryness at 0.1 mm Hg. The residue was dissolved in ether, washed with H2O, dried over MgSO4 and the solvent was removed by distillation under reduced pressure. The oily residue which was not further purified showed in the infrared spectrum a strong carbonyl band at 1730 cm-1.

후처리

  1. temperatureThe solution was cooled
  2. filtrationfiltered with suction
  3. customto remove the precipitate
  4. customthe filtrate was evaporated to dryness at 0.1 mm Hg
  5. dissolutionThe residue was dissolved in ether
  6. washwashed with H2O
  7. dry with materialdried over MgSO4
  8. customthe solvent was removed by distillation under reduced pressure
  9. customThe oily residue which was not further purified

출처 및 근거

ORD 기록
ord-e8ab5674cd3d4f94abe457b6bc99f456
출처 데이터셋
uspto-grants-1978_07
특허 번호
US04098815

반응 노트

불러오는 중…