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Diethyl Ether → HCID 131722977、化合物

HRID 428818
ノート
印刷プレビュー

反応式

HRID 428818 の反応式
[OH:1][C:2]([CH3:23])([CH2:19][CH2:20][CH2:21][CH3:22])[CH2:3]/[CH:4]=[CH:5]/[Sn](CCCC)(CCCC)CCCC.C(OCC)C.C[Li].[Cu]C#N.[Si:34]([O:41][CH:42]1[CH2:46][C:45](=[O:47])[C:44]([CH2:48][CH2:49][CH2:50][CH2:51][CH2:52][CH2:53][C:54]([O:56][CH3:57])=[O:55])=[CH:43]1)([C:37]([CH3:40])([CH3:39])[CH3:38])([CH3:36])[CH3:35].[Cl-].[NH4+]>O1CCCC1>[CH3:57][O:56][C:54](=[O:55])[CH2:53][CH2:52][CH2:51][CH2:50][CH2:49][CH2:48][C@@H:44]1[C@@H:43](/[CH:5]=[CH:4]/[CH2:3][C:2]([OH:1])([CH3:23])[CH2:19][CH2:20][CH2:21][CH3:22])[CH:42]([O:41][Si:34]([C:37]([CH3:40])([CH3:39])[CH3:38])([CH3:35])[CH3:36])[CH2:46][C:45]1=[O:47]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

8

反応物 6

HCID 3283Diethyl EtherHCID 25517Ammonium ChlorideHCID 4653916Methyl 7-(3-((tert-butyldimethylsilyl)oxy)-5-oxocyclopent-1-en-1-yl)heptanoateHCID 11026395HCID 11026395、化合物HCID 178418348HCID 178418348、化合物HCID 178418546HCID 178418546、化合物

生成物 1

HCID 131722977
HCID 131722977、化合物
収率 96%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
-40 °C

実験手順

Into a dry flask was placed a solution of [(4RS, 1E)-4-hydroxy-4-methyl-1-octenyl]tri-n-butyltin (1.36 g, 3.15 mmol) in dry tetrahydrofuran (5 ml) under nitrogen atmosphere, and the mixture was cooled to 0° C. To this solution was dropped 5.7 ml (5.99 mmol) of a diethyl ether solution of methyllithium (1.05 mol/liter), and stirring was continued for 1 h, letting the temperature rise gradually to room temperature. After cooling to −40° C., copper (I) cyanide (141 mg, 1.58 mmol) was added and dissolved by letting the temperature rise gradually to 0° C. This reaction liquid was cooled to −78° C. and added with a solution of (±) methyl 7-(3-tert-butyldimethylsilyloxy-5-oxo-1-cyclopentenyl)heptanoate (318 mg, 0.9 mmol) in dry tetrahydrofuran (1.5 ml) was rapidly added. After stirring for 5 min, 20 ml of a saturated aqueous ammonium chloride/aqueous ammonia (9:1) was added, and stirring was continued for 30 min , letting the temperature rise gradually to room temperature. This mixture was extracted with ethyl acetate (80 ml) two times, and the combined organic layer was washed with a saturated aqueous sodium chloride, dried over anhydrous magnesium sulfate, and concentrated in vacuo to remove solvent. The residue was purified by silica gel column chromatography [ethyl acetate/hexane (1/5)] to give 413 mg (96% yield) of (±)-methyl(16RS, 13E)-11-tert-butyldimethylsilyloxy-16-hydroxy-16-methyl-9-oxoprost-13-en-1-oate as a colorless oil. The spectral data of IR and 1H NMR were identical with those of the example 2.

後処理

  1. customInto a dry flask was placed
  2. customgradually to room temperature
  3. dissolutiondissolved
  4. customgradually to 0° C
  5. customThis reaction liquid
  6. temperaturewas cooled to −78° C.
  7. additionwas rapidly added
  8. stirringAfter stirring for 5 min
  9. stirringstirring
  10. waitwas continued for 30 min
  11. customgradually to room temperature
  12. extractionThis mixture was extracted with ethyl acetate (80 ml) two times
  13. washthe combined organic layer was washed with a saturated aqueous sodium chloride
  14. dry with materialdried over anhydrous magnesium sulfate
  15. concentrationconcentrated in vacuo
  16. customto remove solvent
  17. customThe residue was purified by silica gel column chromatography [ethyl acetate/hexane (1/5)]

出典と根拠

ORDレコード
ord-f0c1f8103e414a6897080845d32f0525
出典データセット
uspto-grants-2001_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06313341B1

反応ノート

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