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Triethylamine → (R)-1-(4-amino-3-chloro-5-trifluoromethyl-benzyl)-2-[4-((R)-2-ethoxycarbonyl-pyrrolidin-1-yl)-piperidin-1-yl]-2-oxo-ethyl 4-(2-oxo-1,2,4,5-tetrahydro-1,3-benzodiazepin-3-yl)-piperidine-1-carboxylate

HRID 2267239
ノート
印刷プレビュー

反応式

HRID 2267239 の反応式
CN(C(ON1N=NC2C=CC=CC1=2)=[N+](C)C)C.[B-](F)(F)(F)F.C(N(CC)CC)C.[O:30]=[C:31]1[N:37]([CH:38]2[CH2:43][CH2:42][N:41]([C:44]([O:46][C@@H:47]([C:61]([OH:63])=O)[CH2:48][C:49]3[CH:54]=[C:53]([C:55]([F:58])([F:57])[F:56])[C:52]([NH2:59])=[C:51]([Cl:60])[CH:50]=3)=[O:45])[CH2:40][CH2:39]2)[CH2:36][CH2:35][C:34]2[CH:64]=[CH:65][CH:66]=[CH:67][C:33]=2[NH:32]1.[NH:68]1[CH2:73][CH2:72][CH:71]([N:74]2[CH2:78][CH2:77][CH2:76][C@@H:75]2[C:79]([O:81][CH2:82][CH3:83])=[O:80])[CH2:70][CH2:69]1>CN(C=O)C>[O:30]=[C:31]1[N:37]([CH:38]2[CH2:39][CH2:40][N:41]([C:44]([O:46][C@H:47]([CH2:48][C:49]3[CH:54]=[C:53]([C:55]([F:57])([F:58])[F:56])[C:52]([NH2:59])=[C:51]([Cl:60])[CH:50]=3)[C:61]([N:68]3[CH2:69][CH2:70][CH:71]([N:74]4[CH2:78][CH2:77][CH2:76][C@@H:75]4[C:79]([O:81][CH2:82][CH3:83])=[O:80])[CH2:72][CH2:73]3)=[O:63])=[O:45])[CH2:42][CH2:43]2)[CH2:36][CH2:35][C:34]2[CH:64]=[CH:65][CH:66]=[CH:67][C:33]=2[NH:32]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 8471TriethylamineHCID 2733207O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborateHCID 58202073(R)-2-(4-amino-3-chloro-5-trifluoromethyl-phenyl)-1-carboxy-ethyl 4-(2-oxo-1,2,4,5-tetrahydro-1,3-benzodiazepin-3-yl)-piperidine-1-carboxylateHCID 66942094ethyl (R)-1-piperidin-4-yl-pyrrolidine-2-carboxylate

生成物 1

HCID 16045646
(R)-1-(4-amino-3-chloro-5-trifluoromethyl-benzyl)-2-[4-((R)-2-ethoxycarbonyl-pyrrolidin-1-yl)-piperidin-1-yl]-2-oxo-ethyl 4-(2-oxo-1,2,4,5-tetrahydro-1,3-benzodiazepin-3-yl)-piperidine-1-carboxylate

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

64 mg (0.20 mmol) TBTU and 28 μL (0.20 mmol) triethylamine were added to a solution of 100 mg (0.18 mmol) (R)-2-(4-amino-3-chloro-5-trifluoromethyl-phenyl)-1-carboxy-ethyl 4-(2-oxo-1,2,4,5-tetrahydro-1,3-benzodiazepin-3-yl)-piperidine-1-carboxylate in 1 mL DMF and stirred for 10 min at RT. 45 mg (0.20 mmol) ethyl (R)-1-piperidin-4-yl-pyrrolidine-2-carboxylate were added to the reaction mixture and this was shaken overnight at RT. After filtration through a syringe filter the reaction solution was purified by HPLC without further working up. The fractions containing the product were combined and freeze-dried.

後処理

  1. stirringthis was shaken overnight at RT
  2. filtrationAfter filtration through a syringe
  3. filtrationfilter the reaction solution
  4. customwas purified by HPLC
  5. additionThe fractions containing the product
  6. customfreeze-dried

出典と根拠

ORDレコード
ord-7f2d5ae3ff99456382aaee9269244a3a
出典データセット
uspto-grants-2010_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07858622B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート