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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
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Water → Benfuresate

HRID 27643
ノート
印刷プレビュー

反応式

HRID 27643 の反応式
S(Cl)(Cl)=O.[CH2:5]([S:7]([O:10][C:11]1[CH:16]=[CH:15][C:14](O)=[C:13]([C:18]([CH3:22])([CH3:21])[CH2:19][OH:20])[CH:12]=1)(=[O:9])=[O:8])[CH3:6].O>CN(C)C=O>[CH2:5]([S:7]([O:10][C:11]1[CH:16]=[CH:15][C:14]2[O:20][CH2:19][C:18]([CH3:22])([CH3:21])[C:13]=2[CH:12]=1)(=[O:9])=[O:8])[CH3:6]
参加物反応条件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 962WaterHCID 24386Thionyl ChlorideHCID 233412894-Hydroxy-3-(2-hydroxy-1,1-dimethylethyl)phenyl ethanesulphonate

生成物 1

HCID 3034378Benfuresate収率 69.9%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

反応条件

温度
5 °C

実験手順

Thionyl chloride (4.3 g) was added dropwise to dimethylformamide (13 ml) maintained at about 5° C. To this was quickly added 4-hydroxy-3-(2-hydroxy-1,1-dimethylethyl)phenyl ethanesulphonate (9.5 g) from Example 2 in dimethylformamide (13 ml). The reaction mixture was then heated to 100° C. and maintained at that temperature for 4-5 hours, after which it was cooled and poured into water (100 ml). The oil was extracted with diethyl ether, washed with water, dried over magnesium sulphate and evaporated down to give 6.2 g of a brownish oil.

後処理

  1. temperatureThe reaction mixture was then heated to 100° C.
  2. temperaturemaintained at that temperature for 4-5 hours
  3. temperatureafter which it was cooled
  4. extractionThe oil was extracted with diethyl ether
  5. washwashed with water
  6. dry with materialdried over magnesium sulphate
  7. customevaporated down

出典と根拠

ORDレコード
ord-3dae8ba852554d2e957caec290b2e483
出典データセット
uspto-grants-1980_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04222767

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート