L-Lysine → HCID 67924379、化合物

HRID 1084823ノート

反応式

HRID 1084823 の反応式
[S:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[CH:6]=[CH:7][C:8]([NH:10][C:11]1[CH:19]=[CH:18][CH:17]=[CH:16][C:12]=1[C:13]([OH:15])=[O:14])=[O:9].[NH2:20][C@H:21]([C:27]([OH:29])=[O:28])[CH2:22][CH2:23][CH2:24][CH2:25][NH2:26]>O1CCCC1.O>[NH2:20][C@H:21]([C:27]([OH:29])=[O:28])[CH2:22][CH2:23][CH2:24][CH2:25][NH2:26].[S:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[CH:6]=[CH:7][C:8]([NH:10][C:11]1[CH:19]=[CH:18][CH:17]=[CH:16][C:12]=1[C:13]([OH:15])=[O:14])=[O:9]

参加物

5

反応物 2

HCID 5962L-LysineHCID 3063368HCID 3063368、化合物

生成物 1

HCID 67924379HCID 67924379、化合物収率 67.5%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of 2-[3-(2-thienyl)acrylamido]benzoic acid (500 mg, 1.8 mmol) in tetrahydrofuran (5 ml) was added L-lysine (267 mg, 1.8 mmol) dissolved in water (3 ml). After stirring the mixture at room temperature for 1.5 hour, the solvent was removed, and the residue was triturated with ether to give crystals. After filtering and drying, the crystals were dissolved in water, the insoluble matter was removed and water was distilled off. The residue was crystallized with ether to give pale yellow solids of the desired L-lysine salt (510 mg, yield, 66%). m.p., 208°-213° C.

後処理

  1. customthe solvent was removed
  2. customthe residue was triturated with ether
  3. customto give crystals
  4. filtrationAfter filtering
  5. customdrying
  6. dissolutionthe crystals were dissolved in water
  7. customthe insoluble matter was removed
  8. distillationwater was distilled off
  9. customThe residue was crystallized with ether

出典と根拠

ORDレコード
ord-ec83b9e36015448fbdc19cee50eb30e7
出典データセット
uspto-grants-1991_04
特許番号
US05006548

反応ノート

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