Chlorosulfonic acid → HCID 23051703、化合物

HRID 973965ノート

反応式

HRID 973965 の反応式
[Cl:1][C:2]1[CH:15]=[CH:14][C:13]2[O:12][C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5](=[O:16])[C:4]=2[CH:3]=1.[Cl:17][S:18](O)(=[O:20])=[O:19].[Cl-].[Ca+2].[Cl-]>>[Cl:17][S:18]([C:8]1[CH:9]=[CH:10][C:11]2[O:12][C:13]3[C:4](=[CH:3][C:2]([Cl:1])=[CH:15][CH:14]=3)[C:5](=[O:16])[C:6]=2[CH:7]=1)(=[O:20])=[O:19]

参加物

4

反応物 3

HCID 24638Chlorosulfonic acidHCID 2555962-Chloro-9-xanthenoneHCID 5284359Calcium Chloride

生成物 1

HCID 23051703HCID 23051703、化合物収率 98.1%

反応条件

温度
120 °C

実験手順

80 g (0.347 moles) of 2-chloroxanthone (DHAR, J. Chem. Soc. 117, 1068) are suspended in 210 ml of chlorosulfonic acid (368.1 g; 3.16 moles) in a 500 ml one neck flask provided with refluxing coolant and calcium chloride valve. The mixture is slowly heated in an oil bath up to 120° C. under magnetic stirring. It is maintained at 120°-130° C. until the gas development ceases (2-3 h). The cool reaction mixture is carefully dropwise added to a becker containing ground ice under mechanical stirring. A heavy crystalline product is separated which is filtered on Buchner and washed with iced H2O. It is dried in air. There are obtained 112 g (98%) of raw 2-(chlorosulfonyl) 7-chloroxanthone. After TLC monitoring (silica gel F245 ; toluene, acetic acid 14:1, visualizer UV) the product is used as such for the next reaction.

後処理

  1. customprovided
  2. temperatureIt is maintained at 120°-130° C. until the gas development ceases (2-3 h)
  3. customThe cool reaction mixture
  4. additionis carefully dropwise added to a becker
  5. additioncontaining ground ice under mechanical stirring
  6. customA heavy crystalline product is separated which
  7. filtrationis filtered on Buchner
  8. washwashed with iced H2O
  9. customIt is dried in air

出典と根拠

ORDレコード
ord-358aacb4ffa345388911f46f0eef9ee6
出典データセット
uspto-grants-1991_11
特許番号
US05066676

反応ノート

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