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Sodium Chloride → HCID 22877878、化合物

HRID 1488849
ノート
印刷プレビュー

反応式

HRID 1488849 の反応式
[NH2:1][C:2]1[CH:3]=[C:4](/[CH:10]=[CH:11]\[C:12]2[CH:17]=[C:16]([O:18][CH3:19])[C:15]([O:20][CH3:21])=[C:14]([O:22][CH3:23])[CH:13]=2)[CH:5]=[CH:6][C:7]=1[O:8][CH3:9].C([NH:41][C@H:42]([C:44]([NH2:46])=[O:45])[CH3:43])(OCC1C2C(=CC=CC=2)C2C1=CC=CC=2)=O.[OH-].[Na+].[Cl-].[Na+]>CO>[NH2:1][C:2]1[CH:3]=[C:4](/[CH:10]=[CH:11]\[C:12]2[CH:13]=[C:14]([O:22][CH3:23])[C:15]([O:20][CH3:21])=[C:16]([O:18][CH3:19])[CH:17]=2)[CH:5]=[CH:6][C:7]=1[O:8][CH3:9].[NH2:41][C@H:42]([C:44]([NH2:46])=[O:45])[CH3:43]
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 3

HCID 5234Sodium ChlorideHCID 14798Sodium HydroxideHCID 22877914HCID 22877914、化合物

生成物 1

HCID 22877878HCID 22877878、化合物収率 87.9%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

One gram (1.6 mmols) of (Z)-1-(3-amino-4-methoxyphenyl)-2-(3,4,5-trimethoxyphenyl)-ethene-Fmoc-L-alanineamide was dissolved in 10 ml of methanol, and 0.9 ml (1.76 mmols) of an aqueous solution of 2-N sodium hydroxide were added thereto. The mixture was stirred for 3 hours. A saturated aqueous solution of sodium chloride was added thereto, and the resulting mixture was extracted three times with dichloromethane. The extract was dried over anhydrous sodium sulfate, and concentrated to dryness under reduced pressure. The product was purified using a silica-gel plate (mixture of 5-% by volume methanol and dichloromethane) to produce 543 mg of the final compound in a yield of 87.9%.

後処理

  1. extractionthe resulting mixture was extracted three times with dichloromethane
  2. dry with materialThe extract was dried over anhydrous sodium sulfate
  3. concentrationconcentrated to dryness under reduced pressure
  4. customThe product was purified
  5. additiona silica-gel plate (mixture of 5-% by volume methanol and dichloromethane)

出典と根拠

ORDレコード
ord-548e0c024d0442089c014ce5294f8304
出典データセット
uspto-grants-1997_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05674906

反応ノート

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