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Hydrochloric Acid → HCID 86712676、化合物

HRID 1779025
ノート
印刷プレビュー

反応式

HRID 1779025 の反応式
C[O:2][C:3](=O)[CH2:4][C:5]1[CH:42]=[CH:41][C:40]([C:43]([F:46])([F:45])[F:44])=[CH:39][C:6]=1[CH2:7][CH2:8][C:9]1[C:14]([C:15]([F:18])([F:17])[F:16])=[CH:13][N:12]=[C:11]([NH:19][C:20]2[CH:25]=[CH:24][C:23]([CH:26]3[CH2:31][CH2:30][N:29]([C:32]([O:34][C:35]([CH3:38])([CH3:37])[CH3:36])=O)[CH2:28][CH2:27]3)=[CH:22][CH:21]=2)N=1.O[Li].[OH2:50].C1C=CC2N(O)N=NC=2C=1.CCN=C=NCCCN(C)C.Cl.Cl.CCN(C(C)C)C(C)C.C(=O)([O-])[O-].[NH4+:87].[NH4+:88]>CO.O.C1COCC1.CCOC(C)=O>[NH2:87][C:3](=[O:2])[CH2:4][C:5]1[CH:42]=[CH:41][C:40]([C:43]([F:44])([F:45])[F:46])=[CH:39][C:6]=1[CH2:7][CH2:8][C:9]1[C:14]([C:15]([F:18])([F:17])[F:16])=[CH:13][N:12]=[C:11]([NH:19][C:20]2[CH:25]=[CH:24][C:23]([CH:26]3[CH2:31][CH2:30][N:29]([C:32]([O:34][C:35]([CH3:38])([CH3:37])[CH3:36])=[O:50])[CH2:28][CH2:27]3)=[CH:22][CH:21]=2)[N:88]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

12

反応物 7

HCID 313Hydrochloric Acid2 回HCID 757711-Hydroxybenzotriazole2 回HCID 81531Diisopropylethylamine2 回HCID 168937Lithium hydroxide, monohydrate2 回HCID 517111Ammonium Carbonate2 回HCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride2 回
HCID 86712675
HCID 86712675、化合物
2 回

生成物 1

HCID 86712676HCID 86712676、化合物

試薬・触媒・溶媒 4

HCID 887Methanol溶媒2 回HCID 962Water溶媒2 回HCID 8028Tetrahydrofuran溶媒3 回HCID 8857Ethyl Acetate溶媒

反応条件

温度
40 °C

実験手順

A suspension of tert-butyl 4-(4-((4-(2-(2-methoxy-2-oxoethyl)-5-(trifluoromethyl)phenethyl)-5-(trifluoromethyl)pyrimidin-2-yl)amino)phenyl)piperidine-1-carboxylate (A61) (0.100 g, 0.150 mmol) and LiOH.H2O (0.051 g, 1.21 mmol) in MeOH (2 mL), water (2 mL) and THF (2 mL) was heated at 40° C. for 16 hours. In a separate flask, a suspension of tert-butyl 4-(4-((4-(2-(2-methoxy-2-oxoethyl)-5-(trifluoromethyl)phenethyl)-5-(trifluoromethyl)pyrimidin-2-yl)amino)phenyl)piperidine-1-carboxylate (A61) (0.070 g, 0.105 mmol) and LiOH.H2O (0.036 g, 0.858 mmol) in MeOH (2 mL), water (2 mL) and THF (2 mL) was heated at 40° C. for 16 hours. The resulting mixtures were combined and the volatiles were removed under reduced pressure. The resulting solid was dissolved in dry DMF (5 mL) and dry THF (5 mL) and HOBt (0.053 g, 0.398 mmol), EDCl.HCl (0.061 g, 0.398 mmol), DIPEA (0.260 mL, 1.53 mmol) and ammonium carbonate (0.144 g, 1.53 mmol) were added. The resulting mixture was stirred at room temperature for 16 hours then HOBt (0.053 g, 0.398 mmol), EDCl.HCl (0.061 g, 0.398 mmol), DIPEA (0.260 mL, 1.53 mmol) and ammonium carbonate (0.144 g, 1.53 mmol) were added and stirring was continued overnight. The resulting mixture was diluted with EtOAc, then washed with 10% aqueous NaHCO3. The organic layer was dried (MgSO4) and the volatiles were removed in vacuo. The resulting solid was adsorbed onto silica gel then purified by column chromatography (Biotage Isolera, SiO2 cartridge, 0-50% EtOAc in petroleum benzine 40-60° C.) to give the title compound A62 as a yellow solid (0.086 g, 43%); 1H NMR (400 MHz, CDCl3) δ 8.54 (s, 1H), 7.55-7.47 (m, 5H), 7.38 (d, J=8.3 Hz, 1H), 7.21 (d, J=8.5 Hz, 2H), 5.48-5.28 (m, 2H), 4.39-4.15 (m, 2H), 3.74 (s, 2H), 3.22-3.13 (m, 2H), 3.12-3.05 (m, 2H), 2.88-2.73 (m, 2H), 2.70-2.56 (m, 1H), 1.85-1.80 (m, 2H), 1.70-1.61 (m, 2H), 1.49 (s, 9H). LCMS-A: rt 6.646 min; m/z 652 [M+H]+.

後処理

  1. temperaturewas heated at 40° C. for 16 hours
  2. customthe volatiles were removed under reduced pressure
  3. dissolutionThe resulting solid was dissolved in dry DMF (5 mL)
  4. stirringstirring
  5. waitwas continued overnight
  6. washwashed with 10% aqueous NaHCO3
  7. dry with materialThe organic layer was dried (MgSO4)
  8. customthe volatiles were removed in vacuo
  9. customthen purified by column chromatography (Biotage Isolera, SiO2 cartridge, 0-50% EtOAc in petroleum benzine 40-60° C.)

出典と根拠

ORDレコード
ord-c227c1108b114fb4a8b37cead6be6395
出典データセット
uspto-grants-2016_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09266864B2

反応ノート

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