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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 → HCID 15917442、化合物

HRID 648097
ノート
印刷プレビュー

反応式

HRID 648097 の反応式
[Cl:1][C:2]1[CH:28]=[CH:27][C:5]2[CH2:6][C:7]3([O:26][C:4]=2[CH:3]=1)[C:16]1[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=1)[CH2:10][N:9](C(OC1C=CC=CC=1)=O)[CH2:8]3.[OH-].[K+].O>C(O)CC>[ClH:1].[Cl:1][C:2]1[CH:28]=[CH:27][C:5]2[CH2:6][C:7]3([O:26][C:4]=2[CH:3]=1)[C:16]1[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=1)[CH2:10][NH:9][CH2:8]3
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 3

HCID 962Water2 回HCID 14797Potassium HydroxideHCID 15917440HCID 15917440、化合物

生成物 1

HCID 15917442HCID 15917442、化合物収率 137.3%

試薬・触媒・溶媒 1

HCID 10311-Propanol溶媒

実験手順

A mixture of 6-chloro-2'-phenoxycarbonylspiro[benzofuran-2(3H),4'(2'H)-isoquinoline] (25.0 g), potassium hydroxide (25 g) and water (25 ml) in n-propanol (250 ml) is heated under reflux for four hours. Removal of the solvent under reduced pressure yields a solid which is stirred with water (500 ml) and extracted with ether. The combined ether extract is washed with 3 N hydrochloric acid and basified with saturated sodium carbonate solution. The material which separates is extracted with ether, washed with saturated sodium chloride solution and dried over anhydrous magnesium sulfate. After filtering, the solvent is removed to yield product as a solid (13.5 g, 78%). A 4.0 g portion of the solid is dissolved in ether and converted to the product hydrochloride salt (4.3 g). An analytical sample is twice recrystallized from ethyl acetate/methanol, mp 238°-239° (dec).

後処理

  1. temperatureis heated
  2. temperatureunder reflux for four hours
  3. customRemoval of the solvent under reduced pressure
  4. customyields a solid which
  5. extractionextracted with ether
  6. extractionThe combined ether extract
  7. washis washed with 3 N hydrochloric acid and basified with saturated sodium carbonate solution
  8. extractionThe material which separates is extracted with ether
  9. washwashed with saturated sodium chloride solution
  10. dry with materialdried over anhydrous magnesium sulfate
  11. filtrationAfter filtering
  12. customthe solvent is removed

出典と根拠

ORDレコード
ord-a6e5c2df70c147c1a42bf96f22d50cb2
出典データセット
uspto-grants-1983_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04410699

反応ノート

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