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Sodium Bicarbonate → 7-Methanesulphonamido-1,2,4,5-tetrahydro-3H-3-benzazepine

HRID 329381
ノート
印刷プレビュー

反応式

HRID 329381 の反応式
C(OC([N:8]1[CH2:14][CH2:13][C:12]2[CH:15]=[CH:16][C:17]([NH:19][S:20]([CH3:23])(=[O:22])=[O:21])=[CH:18][C:11]=2[CH2:10][CH2:9]1)=O)(C)(C)C.C(=O)(O)[O-].[Na+]>C(O)=O>[CH3:23][S:20]([NH:19][C:17]1[CH:16]=[CH:15][C:12]2[CH2:13][CH2:14][NH:8][CH2:9][CH2:10][C:11]=2[CH:18]=1)(=[O:21])=[O:22]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 516892Sodium BicarbonateHCID 187652003-Tertiary-butoxycarbonyl-7-methanesulphonamido-1,2,4,5-tetrahydro-3H-3-benzazepine

生成物 1

HCID 187651877-Methanesulphonamido-1,2,4,5-tetrahydro-3H-3-benzazepine

試薬・触媒・溶媒 1

HCID 284Formic Acid溶媒

実験手順

3-Tertiary-butoxycarbonyl-7-methanesulphonamido-1,2,4,5-tetrahydro-3H-3-benzazepine (0.6 g) and 98% formic acid (10 ml) were stirred together at room temperature for 2 hours. The solvent was evaporated in vacuo to give an oil which was basified with aqueous sodium bicarbonate. The aqueous solution was evaporated in vacuo and the residue was triturated with hot isopropanol. The isopropanol was decanted and evaporated in vacuo to give a solid which was recrystallised from ethyl acetate/hexane to give the title compound, yield 0.22 g.

後処理

  1. customThe solvent was evaporated in vacuo
  2. customto give an oil which
  3. customThe aqueous solution was evaporated in vacuo
  4. customthe residue was triturated with hot isopropanol
  5. customThe isopropanol was decanted
  6. customevaporated in vacuo
  7. customto give a solid which
  8. customwas recrystallised from ethyl acetate/hexane

出典と根拠

ORDレコード
ord-909eaa2493114a61a056d45996e32ebe
出典データセット
uspto-grants-1990_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04891372

反応ノート

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