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Methanol → HCID 58452437、化合物

HRID 70575
ノート
印刷プレビュー

反応式

HRID 70575 の反応式
[H-].C[O:3]CCO[Al+]OCCOC.[Na+].[H-].[Br:15][C:16]1[CH:21]=[CH:20][C:19]([S:22][CH:23]2[CH2:25][CH2:24]2)=[C:18]([Cl:26])[CH:17]=1.CO.[OH2:29]>O1CCCC1>[Br:15][C:16]1[CH:21]=[CH:20][C:19]([S:22]([CH:23]2[CH2:24][CH2:25]2)(=[O:3])=[O:29])=[C:18]([Cl:26])[CH:17]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 887MethanolHCID 962Water2 回HCID 21584525Sodium bis(2-methoxyethoxy)aluminiumhydride2 回HCID 58452584HCID 58452584、化合物

生成物 1

HCID 58452437HCID 58452437、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Oxone(R) (20.3 g) was added to a solution of 4-bromo-2-chloro-1-(cyclopropylsulfanyl)benzene obtained in Reference Example 5-22 (964 mg) in tetrahydrofuran (20 mL)-methanol (20 mL)-water (10 mL), and the mixture was stirred at room temperature for one day. Oxone(R) (6.8 g) was further added and the mixture was stirred at room temperature for 18 hours. Water was added to the reaction solution, followed by extraction with chloroform. The organic layer was dried over anhydrous magnesium sulfate and filtered. The solvent was then evaporated under reduced pressure. The residue was purified by silica gel column chromatography (chloroform only) to give the title compound as a pale yellow amorphous (597 mg, 55%).

後処理

  1. stirringthe mixture was stirred at room temperature for 18 hours
  2. extractionfollowed by extraction with chloroform
  3. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  4. filtrationfiltered
  5. customThe solvent was then evaporated under reduced pressure
  6. customThe residue was purified by silica gel column chromatography (chloroform only)

出典と根拠

ORDレコード
ord-8bcaa7ff2ea546a39b6e4c98f3640ab5
出典データセット
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08822503B2

反応ノート

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