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Ethyl 2-(chloromethyl)-1,4-dithiaspiro[4.4]nonane-7-acetate → Ethyl 2-[(acetylthio)methyl]-1,4-dithiaspiro[4.4]nonane-7-acetate

HRID 1608270
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HRID 1608270 반응식
[C:1]([O-:4])(=[S:3])[CH3:2].[K+].Cl[CH2:7][CH:8]1[CH2:12][S:11][C:10]2([CH2:16][CH2:15][CH:14]([CH2:17][C:18]([O:20][CH2:21][CH3:22])=[O:19])[CH2:13]2)[S:9]1>CN(C=O)C.O>[C:1]([S:3][CH2:7][CH:8]1[CH2:12][S:11][C:10]2([CH2:16][CH2:15][CH:14]([CH2:17][C:18]([O:20][CH2:21][CH3:22])=[O:19])[CH2:13]2)[S:9]1)(=[O:4])[CH3:2]
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참가 물질

5

반응물 2

HCID 19849019Ethyl 2-(chloromethyl)-1,4-dithiaspiro[4.4]nonane-7-acetateHCID 23670855Potassium ethanethioate

생성물 1

HCID 19849041Ethyl 2-[(acetylthio)methyl]-1,4-dithiaspiro[4.4]nonane-7-acetate수율 103.5%

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

A mixture of potassium thioacetate (5.4 g, 0.047 mole) and a solution of the product of Example E (4.0 g, 0.013 mole) in DMF (40 ml) was stirred under nitrogen for 2 days at room temperature. The reaction mixture was diluted with water (200 ml) and extracted twice with ethyl acetate. The organic phase was washed with brine and dried (Na2SO4). The drying agent was filtered and the filtrate stripped on the rotary evaporator to give 4.5 g of the titled compound. This material was a single spot on TLC.

후처리

  1. extractionextracted twice with ethyl acetate
  2. washThe organic phase was washed with brine
  3. dry with materialdried (Na2SO4)
  4. filtrationThe drying agent was filtered
  5. customthe filtrate stripped on the rotary evaporator

출처 및 근거

ORD 기록
ord-e35f119e13b94615b84063cee5bb302d
출처 데이터셋
uspto-grants-1989_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04870098

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