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Water → HCID 12628430、化合物

HRID 1448894
ノート
印刷プレビュー

反応式

HRID 1448894 の反応式
[Cl:1][C:2]1[CH:10]=[CH:9][C:8]2[N:7]([CH3:11])[C:6]3[C:12](=[O:21])[CH:13]=[C:14]([C:16]([O:18]CC)=[O:17])[O:15][C:5]=3[C:4]=2[CH:3]=1.O>C(O)(=O)C.Cl>[Cl:1][C:2]1[CH:10]=[CH:9][C:8]2[N:7]([CH3:11])[C:6]3[C:12](=[O:21])[CH:13]=[C:14]([C:16]([OH:18])=[O:17])[O:15][C:5]=3[C:4]=2[CH:3]=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 2

HCID 962WaterHCID 12628413Ethyl 8-chloro-4,5-dihydro-5-methyl-4-oxopyrano[3,2-b]indole-2-carboxylate

生成物 1

HCID 12628430HCID 12628430、化合物

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 313Hydrochloric Acid溶媒

実験手順

A mixture of 3.5 g (0.012 mole) of ethyl 8-chloro-4,5-dihydro-5-methyl-4-oxopyrano[3,2-b]indole-2-carboxylate in 50 ml glacial acetic acid and 10 ml conc. hydrochloric acid was stirred at reflux for 3 hr, then cooled and added to 500 g ice--H2O. The crude product was filtered, washed with 50% aqueous ethanol, and air dried. A suspension of the product in 75 ml of chloroform was stirred for 90 min at room temperature, then filtered. After recrystallization twice from DMF-water, the final product was dried for several hours under high vacuum at 100°. The yellow flakes obtained had a mpt. of 290°-dec.

後処理

  1. temperatureat reflux for 3 hr
  2. temperaturecooled
  3. filtrationThe crude product was filtered
  4. washwashed with 50% aqueous ethanol, and air
  5. customdried
  6. additionA suspension of the product in 75 ml of chloroform
  7. stirringwas stirred for 90 min at room temperature
  8. filtrationfiltered
  9. customAfter recrystallization twice from DMF-water
  10. dry with materialthe final product was dried for several hours under high vacuum at 100°
  11. customThe yellow flakes obtained
  12. customof 290°

出典と根拠

ORDレコード
ord-12c559f2298141399aad9d6a59199c16
出典データセット
uspto-grants-1980_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04188326

反応ノート

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