ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

p-Chlorothiophenol → (4-Chlorophenyl)(2,5-difluorobenzyl)sulfane

HRID 748665
ノート
印刷プレビュー

反応式

HRID 748665 の反応式
C(=O)([O-])[O-].[K+].[K+].Br[CH2:8][C:9]1[CH:14]=[C:13]([F:15])[CH:12]=[CH:11][C:10]=1[F:16].[Cl:17][C:18]1[CH:23]=[CH:22][C:21]([SH:24])=[CH:20][CH:19]=1.[Cl-].[NH4+]>CN(C)C=O.O>[Cl:17][C:18]1[CH:23]=[CH:22][C:21]([S:24][CH2:8][C:9]2[CH:14]=[C:13]([F:15])[CH:12]=[CH:11][C:10]=2[F:16])=[CH:20][CH:19]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 7815p-ChlorothiophenolHCID 11430Potassium CarbonateHCID 25517Ammonium ChlorideHCID 5228302-(Bromomethyl)-1,4-difluorobenzene

生成物 1

HCID 16681304(4-Chlorophenyl)(2,5-difluorobenzyl)sulfane

試薬・触媒・溶媒 2

HCID 962Water溶媒
HCID 6228
Dimethylformamide
溶媒

実験手順

Process 2: After addition of potassium carbonate (4.00 g, 29.0 mmol) and 2-bromomethyl-1,4-difluorobenzene (5.00 g, 24.2 mmol) to a solution of 4-chlorobenzenethiol (3.86 g, 26.6 mmol) in N,N-dimethylformamide (120 ml), the mixture was stirred for 3 hours at room temperature. To the reaction mixture were added saturated ammonium chloride (50 ml) and water (20 ml), followed by extraction with diethyl ether. The extracts were combined, washed with water and brine, dried over MgSO4, and concentrated. The residue thus obtained was purified by chromatography on a silica gel column (1% ethyl acetate-hexane), whereby the title compound (6.41 g, 98%) was obtained as a colorless oil.

後処理

  1. extractionfollowed by extraction with diethyl ether
  2. washwashed with water and brine
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated
  5. customThe residue thus obtained
  6. customwas purified by chromatography on a silica gel column (1% ethyl acetate-hexane), whereby the title compound (6.41 g, 98%)
  7. customwas obtained as a colorless oil

出典と根拠

ORDレコード
ord-e849e1f639d04014a83c817be3fa06c3
出典データセット
uspto-grants-2008_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07399775B2

反応ノート

読み込み中…

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