Hydrochloric Acid → HCID 9888011、化合物

HRID 1004122

反応式

HRID 1004122 の反応式
[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

参加物

6

反応物 4

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

生成物 1

HCID 9888011HCID 9888011、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒3 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-c2c30a8897d44b19871b8e822c77a7bb
出典データセット
uspto-grants-2000_04
特許番号
US06048875

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