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Diethyl Ether → HCID 14480067, 화합물

HRID 326418
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HRID 326418 반응식
CCOCC.Br[CH2:7][C:8]#[C:9][CH2:10][C:11]#[C:12][CH2:13][C:14]#[C:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH3:23].[CH2:24]([NH:26][C:27](=[O:30])[CH2:28][SH:29])[CH3:25]>C(Cl)Cl>[CH2:24]([NH:26][C:27](=[O:30])[CH2:28][S:29][CH2:7][C:8]#[C:9][CH2:10][C:11]#[C:12][CH2:13][C:14]#[C:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH3:23])[CH3:25]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 3283Diethyl EtherHCID 12736265N-Ethyl-2-sulfanylacetamideHCID 14480083HCID 14480083, 화합물

생성물 1

HCID 14480067HCID 14480067, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

The ether solution of 1-bromo-2,5,8-heptadecatriyne, prepared according to the above operating procedure, is added dropwise under an inert atmosphere to a stirred solution, at 0° C., of sodium thiolate of N-ethylthioglycolamide prepared according to operating procedure b) above. The mixture obtained is stirred for 1 hour after the addition is finished. The solvents are then removed by evaporation under vacuum. The product obtained is dissolved in 100 cm3 of methylene chloride. The organic phase is washed with water, dried over magnesium sulphate, concentrated and then deposited onto a silica gel column. The expected amide is eluted with a mixture of methylene chloride and ethyl acetate (97-3). After evaporation of the eluent, 6 g of product are isolated and are recrystallized from isopropyl ether. 4 g of N-ethyl 3-thia-5,8,11-eicosatriynamide are obtained in the form of beige crystals having a melting point of 59° C.

후처리

  1. customprepared
  2. customThe mixture obtained
  3. additionafter the addition
  4. customThe solvents are then removed by evaporation under vacuum
  5. customThe product obtained
  6. washThe organic phase is washed with water
  7. dry with materialdried over magnesium sulphate
  8. concentrationconcentrated
  9. washThe expected amide is eluted with a mixture of methylene chloride and ethyl acetate (97-3)
  10. customAfter evaporation of the eluent, 6 g of product
  11. customare isolated
  12. customare recrystallized from isopropyl ether

출처 및 근거

ORD 기록
ord-1e8bcf824f054058b353b6dfa5b0b7ed
출처 데이터셋
uspto-grants-1993_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05268494

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