Hydrochloric Acid → HCID 12929143、化合物

HRID 894214ノート

反応式

HRID 894214 の反応式
C([NH:3][CH:4]1[C:10]2[CH:11]=[CH:12][CH:13]=[CH:14][C:9]=2[CH2:8][O:7][C:6]2[CH:15]=[CH:16][C:17]([C:19]([O:21][CH3:22])=[O:20])=[CH:18][C:5]1=2)=O.[ClH:23]>O1CCOCC1>[ClH:23].[NH2:3][CH:4]1[C:10]2[CH:11]=[CH:12][CH:13]=[CH:14][C:9]=2[CH2:8][O:7][C:6]2[CH:15]=[CH:16][C:17]([C:19]([O:21][CH3:22])=[O:20])=[CH:18][C:5]1=2

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 21162715HCID 21162715、化合物

生成物 1

HCID 12929143HCID 12929143、化合物

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

反応条件

温度
40 °C

実験手順

Add 600 mg. of methyl 6,11-dihydro-11-formamidodibenz[b,e]oxepin-2-carboxylate to a mixture of 20 ml. of dioxane and 24 ml. of 10% hydrochloric acid. Stir and heat the mixture at 40° C. for 18 hours. Strip to dryness and triturate the residue in tetrahydrofuran. Separate the solids by filtration. Dissolve the solids in water and basify with aqueous sodium hydroxide. Extract into ether, dry over anhydrous sodium sulfate and filter. Bubble gaseous hydrogen chloride through the solution for 15 minutes and separate the solids. Triturate in tetrahydrofuran and filter to obtain the title product (m.p. 224° C. dec.).

後処理

  1. additionAdd 600 mg
  2. customStrip to dryness and triturate the residue in tetrahydrofuran
  3. customSeparate the solids
  4. filtrationby filtration
  5. dissolutionDissolve the solids in water
  6. extractionExtract into ether
  7. dry with materialdry over anhydrous sodium sulfate
  8. filtrationfilter
  9. customseparate the solids
  10. customTriturate in tetrahydrofuran
  11. filtrationfilter

出典と根拠

ORDレコード
ord-3b39756c9a404c82a095e9836424f92a
出典データセット
uspto-grants-1981_08
特許番号
US04282365

反応ノート

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