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Hydrochloric Acid → Ethyl (7-chloro-2,4-dioxo-3,4-dihydroquinazolin-1(2H)-yl)acetate

HRID 611478
ノート
印刷プレビュー

反応式

HRID 611478 の反応式
[O-:1][C:2]#[N:3].[K+].Cl.S1(CCCC1)(=O)=O.[Cl:13][C:14]1[CH:15]=[C:16]([NH:23][CH2:24][C:25]([O:27][CH2:28][CH3:29])=[O:26])[C:17](=[CH:21][CH:22]=1)[C:18]([OH:20])=O>>[Cl:13][C:14]1[CH:15]=[C:16]2[C:17]([C:18](=[O:20])[NH:3][C:2](=[O:1])[N:23]2[CH2:24][C:25]([O:27][CH2:28][CH3:29])=[O:26])=[CH:21][CH:22]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 4

HCID 313Hydrochloric Acid3 回HCID 31347SulfolaneHCID 111187174-chloro-N-(ethoxycarbonylmethyl)anthranilic acidHCID 11378442Potassium cyanate3 回

生成物 1

HCID 9838691Ethyl (7-chloro-2,4-dioxo-3,4-dihydroquinazolin-1(2H)-yl)acetate収率 95%

実験手順

A total of 128 g of potassium cyanate and 144 g of hydrogen chloride are metered into 700 g of sulfolane at 15-20° C. over a period of 5 hours. For this, 14.4 g of hydrogen chloride are first passed in and 12.8 g of potassium cyanate are then added; this operation is repeated 10 times, until the entire amount of hydrogen chloride and potassium cyanate has been added. 117 g of 4-chloro-N-(ethoxycarbonylmethyl)anthranilic acid are then added at 45-50° C. in the course of 2 hours. The mixture is subsequently stirred for 15 minutes. The suspension is filtered and the residue is washed free from sulfolane and salt with water. After drying, 121 g (95%) of ethyl 1,2,3,4-tetrahydro-7-chloro-2,4-dioxoquinazolin-1-ylacetate are obtained.

後処理

  1. additionare then added
  2. filtrationThe suspension is filtered
  3. washthe residue is washed free from sulfolane and salt with water
  4. customAfter drying

出典と根拠

ORDレコード
ord-2aa50cebd1ab4b7480f8bce0fcaedc70
出典データセット
uspto-grants-1999_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06001831

反応ノート

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