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Methanol → HCID 13827615, 화합물

HRID 235673
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HRID 235673 반응식
[CH:1]1([C:6]2([CH3:22])[CH2:14][C:13]3[C:8](=[C:9]([Cl:20])[C:10]([Cl:19])=[C:11]([S:15]C(=O)C)[CH:12]=3)[C:7]2=[O:21])[CH2:5][CH2:4][CH2:3][CH2:2]1.CO.[OH-].[Na+]>O1CCCC1>[CH:1]1([C:6]2([CH3:22])[CH2:14][C:13]3[C:8](=[C:9]([Cl:20])[C:10]([Cl:19])=[C:11]([SH:15])[CH:12]=3)[C:7]2=[O:21])[CH2:2][CH2:3][CH2:4][CH2:5]1
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참가 물질

5

반응물 3

HCID 887MethanolHCID 14798Sodium HydroxideHCID 13827614(2RS)-2-cyclopentyl-2-methyl-5-acetylthio-6,7-dichloroindan-1-one

생성물 1

HCID 13827615HCID 13827615, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 300 mg of 5-acetylthio compound prepared in (2) in the mixture of 1.3 ml of methanol and 0.6 ml of tetrahydrofuran was dropped 1.35 ml of 5% aqueous solution of sodium hydroxide and the mixture was stirred for 20 minutes at ambient and then concentrated under reduced pressure. 2 ml of water was added to the residue and the mixture was acidified to pH 1 with 1N hydrochloric acid under cooled with ice. The mixture was extracted with diethyl ether and the extract was washed successively with water and a saturated aqueous solution of sodium chloride and dried over anhydrous magnesium sulfate and then concentrated under reduced pressure to give 210 mg of the title compound as crude product having following physical data.

후처리

  1. concentrationthen concentrated under reduced pressure
  2. addition2 ml of water was added to the residue
  3. temperatureunder cooled with ice
  4. extractionThe mixture was extracted with diethyl ether
  5. washthe extract was washed successively with water
  6. dry with materiala saturated aqueous solution of sodium chloride and dried over anhydrous magnesium sulfate
  7. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-efa39192862145bb9f1832c1ccfa7d31
출처 데이터셋
uspto-grants-1987_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04640931

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