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Diethyl Ether → HCID 14480067、化合物

HRID 1886534
ノート
印刷プレビュー

反応式

HRID 1886534 の反応式
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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 3283Diethyl EtherHCID 12736265N-Ethyl-2-sulfanylacetamideHCID 14480083HCID 14480083、化合物

生成物 1

HCID 14480067HCID 14480067、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-98d2d22b71894432a35476a2de60a499
出典データセット
uspto-grants-1992_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05151534

反応ノート

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