Trifluoroacetic acid → (S)-2-(Adamantan-1-ylmethoxycarbonylamino)-3-{[5-(3-guanidino-3-oxo-propyl)-thiophene-2-carbonyl]-amino}-propionic acid

HRID 413221ノート

反応式

HRID 413221 の反応式
C([O:5][C:6](=[O:43])[C@@H:7]([NH:28][C:29]([O:31][CH2:32][C:33]12[CH2:42][CH:37]3[CH2:38][CH:39]([CH2:41][CH:35]([CH2:36]3)[CH2:34]1)[CH2:40]2)=[O:30])[CH2:8][NH:9][C:10]([C:12]1[S:13][C:14]([CH2:17][CH2:18][C:19](=[O:27])[NH:20][C:21]2[NH:22][CH2:23][CH2:24][CH2:25][N:26]=2)=[CH:15][CH:16]=1)=[O:11])(C)(C)C.FC(F)(F)C(O)=O>ClCCl>[C:33]12([CH2:32][O:31][C:29]([NH:28][C@@H:7]([CH2:8][NH:9][C:10]([C:12]3[S:13][C:14]([CH2:17][CH2:18][C:19](=[O:27])[NH:20][C:21]4[NH:22][CH2:23][CH2:24][CH2:25][N:26]=4)=[CH:15][CH:16]=3)=[O:11])[C:6]([OH:43])=[O:5])=[O:30])[CH2:42][CH:37]3[CH2:38][CH:39]([CH2:41][CH:35]([CH2:36]3)[CH2:34]1)[CH2:40]2

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 69637241(2s)-2-(1-Adamantylmethoxycarbonylamino)-3-((5-(2-(1,4,5,6-tetrahydropyrimidin-2-ylcarbamoyl)-ethyl)-thiophene-2-carbonyl)-amino)-propionic acid tert-butyl ester

生成物 1

HCID 10415384(S)-2-(Adamantan-1-ylmethoxycarbonylamino)-3-{[5-(3-guanidino-3-oxo-propyl)-thiophene-2-carbonyl]-amino}-propionic acid

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

117 mg (0.19 mmol) of the product obtained in step c) were dissolved in 5 ml of dichloromethane and stirred for 3 hours with 1 ml of trifluoroacetic acid under an inert gas atmosphere at room temperature. The solvents were removed in vacuo, and the residue was dissolved in acetic acid and again evaporated to dryness. This procedure was repeated once. The resinous residue was triturated with diethyl ether. After filtration 90 mg of a colourless amorphous powder were obtained.

後処理

  1. customThe solvents were removed in vacuo
  2. dissolutionthe residue was dissolved in acetic acid
  3. customagain evaporated to dryness
  4. customThe resinous residue was triturated with diethyl ether
  5. filtrationAfter filtration 90 mg of a colourless amorphous powder
  6. customwere obtained

出典と根拠

ORDレコード
ord-b556143f01c244fbad846c6cfa134994
出典データセット
uspto-grants-2003_05
特許番号
US06566366B1

反応ノート

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