Z-Ala-gln-OH → L-Alanyl-L-Glutamine

HRID 1086941

反応式

HRID 1086941 の反応式
C([NH:11][C@H:12]([C:14]([NH:16][C@H:17]([C:23]([OH:25])=[O:24])[CH2:18][CH2:19][C:20](=[O:22])[NH2:21])=[O:15])[CH3:13])(OCC1C=CC=CC=1)=O.[H][H]>CO.O.[C].[Pd]>[NH2:11][C@H:12]([C:14]([NH:16][C@H:17]([C:23]([OH:25])=[O:24])[CH2:18][CH2:19][C:20](=[O:22])[NH2:21])=[O:15])[CH3:13]

参加物

6

反応物 2

HCID 14534789Z-Ala-gln-OHHCID 178418361HCID 178418361、化合物

生成物 1

HCID 123935L-Alanyl-L-Glutamine収率 90.8%

試薬・触媒・溶媒 3

HCID 178418390HCID 178418390、化合物触媒HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

Into a 200 ml three-necked flask was charged 5.0 g (14.2 mmol) of Z-L-Ala-L-Gln, and the peptide was dissolved in 100 ml of a mixture of methanol and water (methanol:water =7:3) and stirred with a magnetic stirrer. After the air in the flask had been replaced with nitrogen, 0.8 g of 2% by weight of palladium-carbon was added thereto, and the protective group was eliminated in a stream of hydrogen. After 2 hours, the completion of the reaction was confirmed by thin layer chromatography, and then the palladium-carbon was filtered off. The filtrate was concentrated to 20 ml under reduced pressure, and 40 ml of isopropyl alcohol was added thereto. The resulting mixture was stirred for 30 minutes, during which time crystals precipitated. The crystals were collected by filtration, washed with isopropyl alcohol and then dried under reduced pressure to give 2.8 g (12.9 mmol) (90%) of L-Ala-L-Gln.

後処理

  1. additionwas added
  2. filtrationthe palladium-carbon was filtered off
  3. concentrationThe filtrate was concentrated to 20 ml under reduced pressure, and 40 ml of isopropyl alcohol
  4. additionwas added
  5. stirringThe resulting mixture was stirred for 30 minutes, during which time crystals
  6. customprecipitated
  7. filtrationThe crystals were collected by filtration
  8. washwashed with isopropyl alcohol
  9. customdried under reduced pressure

出典と根拠

ORDレコード
ord-60edb0568624431aa3dd8c20db345199
出典データセット
uspto-grants-1991_07
特許番号
US05032675

関連ノート

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