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Hydrochloric Acid → HCID 42878057、化合物

HRID 18115
ノート
印刷プレビュー

反応式

HRID 18115 の反応式
[O:1]=[S:2]1(=[O:16])[C:13]2[C:5](=[C:6]3[C:10](=[CH:11][CH:12]=2)[NH:9]C(=O)[C:7]3=[O:15])[CH2:4][CH2:3]1.[OH-:17].[Na+].OO.Cl>O>[NH2:9][C:10]1[CH:11]=[CH:12][C:13]2[S:2](=[O:1])(=[O:16])[CH2:3][CH2:4][C:5]=2[C:6]=1[C:7]([OH:15])=[O:17]
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 313Hydrochloric AcidHCID 784Hydrogen PeroxideHCID 14798Sodium HydroxideHCID 593450663,3-Dioxo-1,2,3,6-tetrahydro-3lambda6-thieno[3,2-e]indole-7,8-dione

生成物 1

HCID 42878057HCID 42878057、化合物収率 60.6%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
40 °C

実験手順

1.5 g (6.32 mmol) of 3,3-dioxo-1,2,3,6-tetrahydro-3λ6-thieno[3,2-e]indole-7,8-dione were introduced into a 10 ml three-neck round-bottom flask and dissolved in 6.5 ml of 1M (207.2 mmol) sodium hydroxide solution. 1.5 ml (1.32 mmol) of a 30% strength hydrogen peroxide solution were slowly added dropwise over the course of 30 minutes. The internal temperature during the addition was kept between 30-40° C. despite the exothermic reaction. After the addition was complete, the mixture was stirred at 40° C. for 1.5 h. The mixture was then cooled to RT and, after addition to a little water (about 7 ml), acidified with a 10% strength HCl to pH 1, and the precipitated solid was filtered off with suction. The latter was washed successively with water and diethyl ether and dried in vacuo overnight. 870 mg of the desired compound were obtained.

後処理

  1. additionThe internal temperature during the addition
  2. customwas kept between 30-40° C. despite the exothermic reaction
  3. additionAfter the addition
  4. temperatureThe mixture was then cooled to RT
  5. filtrationthe precipitated solid was filtered off with suction
  6. washThe latter was washed successively with water and diethyl ether
  7. customdried in vacuo overnight

出典と根拠

ORDレコード
ord-cc35f39e22f0468dbd1d3986ce7c4cdd
出典データセット
uspto-grants-2010_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07741333B2

反応ノート

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