Hydrochloric Acid → HCID 9888011, 화합물

HRID 1004122

반응식

HRID 1004122 반응식
[CH3:1]C([O-])(C)C.[K+].[Br-].[CH2:8]([O:10][C:11]([CH2:13][P+](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)=[O:12])[CH3:9].[CH3:33][O:34][C:35]1[C:54]([O:55][CH3:56])=[CH:53][C:38]2[S:39][C:40](C=O)=[C:41]([O:42][C:43]3[CH:48]=[CH:47][C:46]([O:49][CH3:50])=[CH:45][CH:44]=3)[C:37]=2[CH:36]=1.Cl>O1CCCC1>[CH3:33][O:34][C:35]1[C:54]([O:55][CH3:56])=[CH:53][C:38]2[S:39][C:40](/[CH:1]=[CH:13]/[C:11]([O:10][CH2:8][CH3:9])=[O:12])=[C:41]([O:42][C:43]3[CH:44]=[CH:45][C:46]([O:49][CH3:50])=[CH:47][CH:48]=3)[C:37]=2[CH:36]=1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 73731(Ethoxycarbonylmethyl)triphenylphosphonium bromideHCID 110892155,6-Dimethoxy-3-(4-methoxyphenoxy)benzo[b]thiophene-2-carbaldehydeHCID 23665647Potassium tert-butoxide

생성물 1

HCID 9888011HCID 9888011, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매3회

실험 절차

20 ml of a 1M solution of potassium tert-butylate in tetrahydrofuran are added dropwise at 0° C. under an inert atmosphere to a suspension of 0.02 mol of (ethoxycarbonylmethyl)triphenylphosphonium bromide in 90 ml of tetrahydrofuran. After the addition is complete and the mixture has returned to room temperature, 0.01 mol of the compound obtained in Step E of Example 1 diluted in 30 ml of tetrahydrofuran is added. After 12 hours, the reaction mixture is hydrolysed by the addition of 100 ml of a 1N HCl solution, and then extracted with ethyl acetate; the combined organic phases are washed with water and then with a saturated NaCl solution, dried over sodium sulphate, filtered and concentrated under reduced pressure. Chromatography over silica gel (pentane/ethyl acetate: 90/10) enables 2.78 g of the expected product to be isolated.

후처리

  1. additionAfter the addition
  2. customhas returned to room temperature
  3. additionis added
  4. extractionextracted with ethyl acetate
  5. washthe combined organic phases are washed with water
  6. dry with materialwith a saturated NaCl solution, dried over sodium sulphate
  7. filtrationfiltered
  8. concentrationconcentrated under reduced pressure
  9. customto be isolated

출처 및 근거

ORD 기록
ord-c2c30a8897d44b19871b8e822c77a7bb
출처 데이터셋
uspto-grants-2000_04
특허 번호
US06048875

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