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

HRID 413218ノート

反応式

HRID 413218 の反応式
C([O:5][C:6](=[O:44])[C@@H:7]([NH:29][C:30]([O:32][CH2:33][C:34]12[CH2:43][CH:38]3[CH2:39][CH:40]([CH2:42][CH:36]([CH2:37]3)[CH2:35]1)[CH2:41]2)=[O:31])[CH2:8][NH:9][C:10]([C:12]1[S:13][C:14]([CH:17]2[CH2:19][CH:18]2[C:20](=[O:28])[NH:21][C:22]2[NH:23][CH2:24][CH2:25][CH2:26][N:27]=2)=[CH:15][CH:16]=1)=[O:11])(C)(C)C.FC(F)(F)C(O)=O>ClCCl>[C:34]12([CH2:33][O:32][C:30]([NH:29][C@@H:7]([CH2:8][NH:9][C:10]([C:12]3[S:13][C:14]([CH:17]4[CH2:19][CH:18]4[C:20](=[O:28])[NH:21][C:22]4[NH:23][CH2:24][CH2:25][CH2:26][N:27]=4)=[CH:15][CH:16]=3)=[O:11])[C:6]([OH:44])=[O:5])=[O:31])[CH2:43][CH:38]3[CH2:39][CH:40]([CH2:42][CH:36]([CH2:37]3)[CH2:35]1)[CH2:41]2

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 69637307(2s)-2-(1-Adamantylmethoxycarbonylamino)-3-((5-(2-(1,4,5,6-tetrahydropyrimidin-2-ylcarbamoyl)-cyclopropyl)-thiophene-2-carbonyl)-amino)-propionic acid tert-butyl ester

生成物 1

HCID 15859414(S)-2-(Adamantan-1-ylmethoxycarbonylamino)-3-{[5-(2-guanidinocarbonyl-cyclopropyl)-thiophene-2-carbonyl]-amino}-propionic acid

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

48 mg of the product obtained in step c) were dissolved in 2 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, the residue was dissolved in acetic acid and the solution was again evaporated to dryness. This procedure was repeated once. The resinous residue was triturated with diethyl ether. After filtration 30 mg of the title compound were obtained as a colourless amorphous powder.

後処理

  1. customThe solvents were removed in vacuo
  2. dissolutionthe residue was dissolved in acetic acid
  3. customthe solution was again evaporated to dryness
  4. customThe resinous residue was triturated with diethyl ether
  5. filtrationAfter filtration 30 mg of the title compound
  6. customwere obtained as a colourless amorphous powder

出典と根拠

ORDレコード
ord-aa151016de1340bbbd73b29089fcaf18
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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