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

Water → {4-[(1,3-Benzothiazol-2-yl)sulfanyl]phenyl}(2,5-dichlorophenyl)methanone

HRID 1666036
ノート
印刷プレビュー

反応式

HRID 1666036 の反応式
[Cl:1][C:2]1[CH:16]=[CH:15][C:14]([Cl:17])=[CH:13][C:3]=1[C:4]([C:6]1[CH:11]=[CH:10][C:9](F)=[CH:8][CH:7]=1)=[O:5].[S:18]1[C:22]2[CH:23]=[CH:24][CH:25]=[CH:26][C:21]=2[N:20]=[C:19]1[SH:27].C(=O)([O-])[O-].[K+].[K+].O>C1(C)C=CC=CC=1>[Cl:1][C:2]1[CH:16]=[CH:15][C:14]([Cl:17])=[CH:13][C:3]=1[C:4]([C:6]1[CH:11]=[CH:10][C:9]([S:27][C:19]2[S:18][C:22]3[CH:23]=[CH:24][CH:25]=[CH:26][C:21]=3[N:20]=2)=[CH:8][CH:7]=1)=[O:5]
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

6

反応物 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 120399992,5-Dichloro-4'-fluorobenzophenonHCID 178418395HCID 178418395、化合物

生成物 1

HCID 59165205{4-[(1,3-Benzothiazol-2-yl)sulfanyl]phenyl}(2,5-dichlorophenyl)methanone収率 78.2%

試薬・触媒・溶媒 1

HCID 1140
Toluene
溶媒

反応条件

温度
110 °C

実験手順

A charge of 269.1 g (1.00 mol) of 2,5-dichloro-4′-fluorobenzophenone, 175.6 g (1.05 mol) of 2-benzothiazolethiol, 152.0 g (1.10 mol) of potassium carbonate and 1.5 L of dehydrated N,N′-dimethylacetamide was weighed into a 3 L three-neck flask equipped with a stirrer, a thermometer, a cooling tube and a nitrogen gas introducing tube. The reaction solution was heated under nitrogen atmosphere to 110° C. for 2 hours using an oil bath. After the disappearance of raw materials was confirmed by thin layer chromatography, the reaction solution was left to cool to room temperature. The reaction solution was then gradually added to 3 L of water to coagulate a product, which was filtered. The product obtained by filtration was dissolved in 4 L of toluene. The organic layer was washed with brine until an aqueous layer became neutral. After the organic layer was dried over magnesium sulfate, the solvent was removed by an evaporator. A crude yield was 350.3 g. A 1.5 L aliquot of toluene heated to 80° C. was used for recrystallization to yield 325.4 g (0.782 mol) of a purified product in 78.2% yield.

後処理

  1. customwas weighed into a 3 L three-neck flask
  2. customequipped with a stirrer
  3. additiona thermometer, a cooling tube and a nitrogen gas introducing tube
  4. waitthe reaction solution was left
  5. temperatureto cool to room temperature
  6. filtrationwas filtered
  7. customThe product obtained by filtration
  8. washThe organic layer was washed with brine until an aqueous layer
  9. dry with materialAfter the organic layer was dried over magnesium sulfate
  10. customthe solvent was removed by an evaporator
  11. temperatureA 1.5 L aliquot of toluene heated to 80° C.
  12. customwas used for recrystallization

出典と根拠

ORDレコード
ord-039caa0b75604ae99b5a864c0a2466dc
出典データセット
uspto-grants-2011_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08043762B2

反応ノート

読み込み中…

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