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Sodium Hydroxide → HCID 21995280、化合物

HRID 1977684
ノート
印刷プレビュー

反応式

HRID 1977684 の反応式
C([O:3][C:4]([CH2:6][C:7]1[CH:12]=[CH:11][C:10]([NH:13][C:14]2[CH:19]=[CH:18][N:17]=[C:16]([NH:20][C:21]3[CH:26]=[C:25]([O:27][CH3:28])[C:24]([O:29][CH3:30])=[C:23]([O:31][CH3:32])[CH:22]=3)[N:15]=2)=[CH:9][CH:8]=1)=[O:5])C.[OH-].[Na+]>C(O)C>[C:4]([CH2:6][C:7]1[CH:8]=[CH:9][C:10]([NH:13][C:14]2[CH:19]=[CH:18][N:17]=[C:16]([NH:20][C:21]3[CH:22]=[C:23]([O:31][CH3:32])[C:24]([O:29][CH3:30])=[C:25]([O:27][CH3:28])[CH:26]=3)[N:15]=2)=[CH:11][CH:12]=1)([OH:5])=[O:3]
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 14798Sodium HydroxideHCID 21995173HCID 21995173、化合物

生成物 1

HCID 21995280HCID 21995280、化合物収率 38%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

The compound of Example 103 (250 mg, 0.57 mmol) in a solution of ethanol (10 ml) containing 6N aqueous NaOH (2.0 ml) was heated a reflux for 2 h. On cooling the ethanol was removed under reduced pressure and the basic solution brought to pH 5 with 2M hydrochloric acid. The resulting solution was concentrated under reduced pressure, and the residue taken up in hot ethanol (20 ml). This solution was filtered and the filtrate evaporated under reduced pressure to give a residue which was crystalised from ethanol to give the title compound (89 mg) as a white solid m.p. 144-150°. MS m/z 411 (M+H)+.

後処理

  1. temperaturewas heated
  2. temperaturea reflux for 2 h
  3. customwas removed under reduced pressure
  4. concentrationThe resulting solution was concentrated under reduced pressure
  5. filtrationThis solution was filtered
  6. customthe filtrate evaporated under reduced pressure
  7. customto give a residue which
  8. customwas crystalised from ethanol

出典と根拠

ORDレコード
ord-a23b4981961e4b07982ff40c14e2d63a
出典データセット
uspto-grants-2001_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06235746B1

反応ノート

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