Sodium Bicarbonate → (3R)-tert-butyl 3-(3,5-difluorophenyl)-5-oxo-4-(2-oxo-2-(2'-oxo-1',2',5,7-tetrahydrospiro[cyclopenta[b]pyridin-6,3'-pyrrolo[2,3-b]pyridin]-3-ylamino)ethyl)-8,11-dioxa-1,4-diaza-spiro[5.6]dodecane-1-carboxylate

HRID 1615758ノート

反応式

HRID 1615758 の反応式
[C:1]([CH2:4][N:5]1[C:10](=[O:11])[C:9]2([CH2:17][O:16][CH2:15][CH2:14][O:13][CH2:12]2)[N:8]([C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19])[CH2:7][C@H:6]1[C:25]1[CH:30]=[C:29]([F:31])[CH:28]=[C:27]([F:32])[CH:26]=1)([OH:3])=O.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.[NH2:57][C:58]1[CH:59]=[C:60]2[CH2:75][C:65]3([C:73]4[C:68](=[N:69][CH:70]=[CH:71][CH:72]=4)[NH:67][C:66]3=[O:74])[CH2:64][C:61]2=[N:62][CH:63]=1.C(=O)([O-])O.[Na+]>CN(C=O)C>[F:32][C:27]1[CH:26]=[C:25]([C@H:6]2[N:5]([CH2:4][C:1](=[O:3])[NH:57][C:58]3[CH:59]=[C:60]4[CH2:75][C:65]5([C:73]6[C:68](=[N:69][CH:70]=[CH:71][CH:72]=6)[NH:67][C:66]5=[O:74])[CH2:64][C:61]4=[N:62][CH:63]=3)[C:10](=[O:11])[C:9]3([CH2:12][O:13][CH2:14][CH2:15][O:16][CH2:17]3)[N:8]([C:18]([O:20][C:21]([CH3:24])([CH3:22])[CH3:23])=[O:19])[CH2:7]2)[CH:30]=[C:29]([F:31])[CH:28]=1

参加物

6

反応物 4

HCID 516892Sodium BicarbonateHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 579740903-amino-5,7-dihydrospiro[cyclopenta-[b]pyridin-6.3'-pyrrolo[2,3-b]pyridin]-2'(1'H)-oneHCID 68154191tert-butyl (R)-4-carboxymethyl-3-(3,5-difluoro-phenyl)-5-oxo-8,11-dioxa-1,4-diaza-spiro[5.6]dodecane-1-carboxylate

生成物 1

HCID 68154406(3R)-tert-butyl 3-(3,5-difluorophenyl)-5-oxo-4-(2-oxo-2-(2'-oxo-1',2',5,7-tetrahydrospiro[cyclopenta[b]pyridin-6,3'-pyrrolo[2,3-b]pyridin]-3-ylamino)ethyl)-8,11-dioxa-1,4-diaza-spiro[5.6]dodecane-1-carboxylate

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

0.13 g (0.28 mmol) tert-butyl (R)-4-carboxymethyl-3-(3,5-difluoro-phenyl)-5-oxo-8,11-dioxa-1,4-diaza-spiro[5.6]dodecane-1-carboxylate in 2 ml DMF were combined with 0.11 g (0.29 mmol) HATU and 0.08 ml (0.60 mmol) TEA and stirred for 3 min at RT. Then 72 mg (0.28 mmol) 3-amino-5,7-dihydrospiro[cyclopenta-[b]pyridin-6.3′-pyrrolo[2,3-b]pyridin]-2′(1′H)-one were added and the mixture was stirred overnight at RT. The reaction mixture was poured onto saturated sodium hydrogen carbonate solution. The precipitate formed was suction filtered, washed with water and dried.

後処理

  1. stirringthe mixture was stirred overnight at RT
  2. customThe precipitate formed
  3. filtrationfiltered
  4. washwashed with water
  5. customdried

出典と根拠

ORDレコード
ord-6fbd4eac41c04364a55d76724c56b438
出典データセット
uspto-grants-2014_07
特許番号
US08765763B2

反応ノート

読み込み中…