Hydrochloric Acid → HCID 12929151、化合物

HRID 894215ノート

反応式

HRID 894215 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]C)=[O:20])=[CH:18][C:5]1=2)=O.O1CCOCC1.[ClH:29]>O>[ClH:29].[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]([OH:21])=[O:20])=[CH:18][C:5]1=2

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 312751,4-DioxaneHCID 21162715HCID 21162715、化合物

生成物 1

HCID 12929151HCID 12929151、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Heat together 340 mg. of methyl 6,11-dihydro-11-formamidodibenz[b,e]oxepin-2-carboxylate, 10 ml. of dioxane and 10 ml. of concentrated hydrochloric acid at 100° C. for 5 hours. Strip to dryness and dissolve the residue in water and pass through a Bio-Red AG-50W-X8 resin (sulfonic acid type). Collect the acid by elution with 10% ammonium hydroxide solution. Evaporate to dryness, dissolve the residue in tetrahydrofuran and acidify with aqueous hydrochloric acid. Strip to dryness and recrystallize from methanol/ether to obtain the title product (m.p. 245° dec.).

後処理

  1. temperatureHeat together 340 mg
  2. customCollect the acid
  3. washby elution with 10% ammonium hydroxide solution
  4. customEvaporate to dryness
  5. dissolutiondissolve the residue in tetrahydrofuran
  6. customStrip to dryness and recrystallize from methanol/ether

出典と根拠

ORDレコード
ord-4a4aed83a9fd4a7fa7a7807944a7e36a
出典データセット
uspto-grants-1981_08
特許番号
US04282365

反応ノート

読み込み中…