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Sodium methanethiolate → HCID 67004755、化合物

HRID 2421516
ノート
印刷プレビュー

反応式

HRID 2421516 の反応式
Br[CH:2]([O:10][C:11]1[CH:16]=[C:15]([Cl:17])[CH:14]=[C:13]([Cl:18])[CH:12]=1)[C:3]([O:5][C:6]([CH3:9])([CH3:8])[CH3:7])=[O:4].[CH3:19][S-:20].[Na+]>O1CCOCC1>[CH3:19][S:20][CH:2]([O:10][C:11]1[CH:16]=[C:15]([Cl:17])[CH:14]=[C:13]([Cl:18])[CH:12]=1)[C:3]([O:5][C:6]([CH3:9])([CH3:8])[CH3:7])=[O:4]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 4378561Sodium methanethiolateHCID 85975967HCID 85975967、化合物

生成物 1

HCID 67004755HCID 67004755、化合物収率 88.1%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

t-Butyl 2-bromo-2-(3,5-dichlorophenoxy)acetate (1.0 g) was dissolved in 1,4-dioxane (3 ml), and sodium thiomethoxide (0.218 g) was added to the mixture. The resulting pale yellow suspension was stirred at ambient temperature for 5 hours and then stored for 18 hours. The solvent was evaporated, water was added and the aqueous layer was extracted twice with ethyl acetate (100 ml). The organic layers were combined, washed with brine, dried over magnesium sulphate, filtered and evaporated to give t-butyl 2-methylthio-2-(3,5-dichlorophenoxy)acetate as a pale yellow solid (0.80 g) which was used in the next step without further purification.

後処理

  1. waitstored for 18 hours
  2. customThe solvent was evaporated
  3. additionwater was added
  4. extractionthe aqueous layer was extracted twice with ethyl acetate (100 ml)
  5. washwashed with brine
  6. dry with materialdried over magnesium sulphate
  7. filtrationfiltered
  8. customevaporated

出典と根拠

ORDレコード
ord-cb09e6808bdb4d3fb328d20faad65a79
出典データセット
uspto-grants-2011_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07956188B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート