Trifluoroacetic acid → 4-[({(2S,4S)-1-[(1-carbamimidoyl-4-piperidinyl)carbonyl]-4-[4-(methylsulfonyl)-1-piperazinyl]-2-pyrrolidinyl}carbonyl)amino]benzoic acid bis(trifluoroacetate)

HRID 1053816ノート

反応式

HRID 1053816 の反応式
CC(OC([NH:8][C:9]([N:18]1[CH2:23][CH2:22][CH:21]([C:24]([N:26]2[CH2:30][C@@H:29]([N:31]3[CH2:36][CH2:35][N:34]([S:37]([CH3:40])(=[O:39])=[O:38])[CH2:33][CH2:32]3)[CH2:28][C@H:27]2[C:41]([NH:43][C:44]2[CH:56]=[CH:55][C:47]([C:48]([O:50]C(C)(C)C)=[O:49])=[CH:46][CH:45]=2)=[O:42])=[O:25])[CH2:20][CH2:19]1)=[N:10]C(OC(C)(C)C)=O)=O)(C)C.[F:57][C:58]([F:63])([F:62])[C:59]([OH:61])=[O:60]>ClCCl>[F:57][C:58]([F:63])([F:62])[C:59]([OH:61])=[O:60].[F:57][C:58]([F:63])([F:62])[C:59]([OH:61])=[O:60].[C:9]([N:18]1[CH2:19][CH2:20][CH:21]([C:24]([N:26]2[CH2:30][C@@H:29]([N:31]3[CH2:36][CH2:35][N:34]([S:37]([CH3:40])(=[O:39])=[O:38])[CH2:33][CH2:32]3)[CH2:28][C@H:27]2[C:41]([NH:43][C:44]2[CH:45]=[CH:46][C:47]([C:48]([OH:50])=[O:49])=[CH:55][CH:56]=2)=[O:42])=[O:25])[CH2:22][CH2:23]1)(=[NH:8])[NH2:10]

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 1317363002-methyl-2-propanyl 4-[({(2S,4S)-1-{[1-(N,N'-bis{[(2-methyl-2-propanyl)oxy]carbonyl}carbamimidoyl)-4-piperidinyl]carbonyl}-4-[4-(methylsulfonyl)-1-piperazinyl]-2-pyrrolidinyl}carbonyl)amino]benzoate

生成物 1

HCID 1181076974-[({(2S,4S)-1-[(1-carbamimidoyl-4-piperidinyl)carbonyl]-4-[4-(methylsulfonyl)-1-piperazinyl]-2-pyrrolidinyl}carbonyl)amino]benzoic acid bis(trifluoroacetate)収率 40%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of the compound prepared in Example 8 (0.11 g, 0.13 mmol) in dichloromethane (15 mL) at 0° C. was added trifluoroacetic acid (0.5 mL). The reaction was warmed to room temperature and stirred for 18 h. The solvent and excess trifluoroacetic acid was removed under reduced pressure. The solid was dissolved in water and lyophilized to dryness to afford the title compound (0.030 g, 40%) as an off-white solid.

後処理

  1. customThe solvent and excess trifluoroacetic acid was removed under reduced pressure
  2. dissolutionThe solid was dissolved in water

出典と根拠

ORDレコード
ord-7593e35dfcb74a7ab3f40c3a06977b27
出典データセット
uspto-grants-2016_07
特許番号
US09394250B2

反応ノート

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