Water → L-methionyl-L-aspartyl-D-alanine amide hydrochloride

HRID 596804ノート

反応式

HRID 596804 の反応式
C(OC([NH:8][C@H:9]([C:14]([NH:16][C@H:17]([C:22]([NH:24][C@@H:25]([C:27]([NH2:29])=[O:28])[CH3:26])=[O:23])[CH2:18][C:19](=[O:21])[OH:20])=[O:15])[CH2:10][CH2:11][S:12][CH3:13])=O)(C)(C)C.O.[ClH:31].O1CCOCC1>C(O)(=O)C>[ClH:31].[NH2:8][C@H:9]([C:14]([NH:16][C@H:17]([C:22]([NH:24][C@@H:25]([C:27]([NH2:29])=[O:28])[CH3:26])=[O:23])[CH2:18][C:19](=[O:20])[OH:21])=[O:15])[CH2:10][CH2:11][S:12][CH3:13]

参加物

5

反応物 3

HCID 962WaterHCID 204431481,4-Dioxane hydrochlorideHCID 22796339N-t-butoxycarbonyl-L-methionyl-L-aspartyl-D-alanine amide

生成物 1

HCID 22796354L-methionyl-L-aspartyl-D-alanine amide hydrochloride

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

12.54 Parts of N-t-butoxycarbonyl-L-methionyl-L-aspartyl-D-alanine amide is dissolved in 107 parts by volume glacial acetic acid and 51.66 parts by volume of a 5.6 M solution of HCl/dioxane. The resultant mixture is stirred for 20 minutes and then stripped under reduced pressure to afford a solid. The solid is triturated with ethyl ether, cooled, and the resultant product washed with cold ethyl ether and vacuum dried. This solid is purified by countercurrent distribution to afford L-methionyl-L-aspartyl-D-alanine amide hydrochloride hydrated with 2/3 mole of water per mole, and represented by the following formula.

後処理

  1. customto afford a solid
  2. customThe solid is triturated with ethyl ether
  3. temperaturecooled
  4. washthe resultant product washed with cold ethyl ether and vacuum
  5. customdried
  6. customThis solid is purified by countercurrent distribution

出典と根拠

ORDレコード
ord-c6ddfcbe70fe4dab9a37bb9b849a37d2
出典データセット
uspto-grants-1977_03
特許番号
US04012367

反応ノート

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