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Pivalic acid → Tert-butyl 3-{1-hydroxy-1-[5-(4-methyl-6-{[4-(trifluoromethyl)-pyridin-2-yl]amino}pyridin-2-yl)-1,3-thiazol-2-yl]ethyl}pyrrolidine-1-carboxylate

HRID 2272675
ノート
印刷プレビュー

反応式

HRID 2272675 の反応式
[OH:1][C:2]([CH:9]1[CH2:13][CH2:12][N:11]([C:14]([O:16][C:17]([CH3:20])([CH3:19])[CH3:18])=[O:15])[CH2:10]1)([C:4]1[S:5][CH:6]=[CH:7][N:8]=1)[CH3:3].Br[C:22]1[N:27]=[C:26]([NH:28][C:29]2[CH:34]=[C:33]([C:35]([F:38])([F:37])[F:36])[CH:32]=[CH:31][N:30]=2)[CH:25]=[C:24]([CH3:39])[CH:23]=1.C(P(C12CC3CC(CC(C3)C1)C2)C12CC3CC(CC(C3)C1)C2)CCC.C(O)(=O)C(C)(C)C.C(=O)([O-])[O-].[K+].[K+]>C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd].CN(C)C(=O)C>[OH:1][C:2]([CH:9]1[CH2:13][CH2:12][N:11]([C:14]([O:16][C:17]([CH3:20])([CH3:19])[CH3:18])=[O:15])[CH2:10]1)([C:4]1[S:5][C:6]([C:22]2[CH:23]=[C:24]([CH3:39])[CH:25]=[C:26]([NH:28][C:29]3[CH:34]=[C:33]([C:35]([F:36])([F:37])[F:38])[CH:32]=[CH:31][N:30]=3)[N:27]=2)=[CH:7][N:8]=1)[CH3:3]
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

8

反応物 5

HCID 6417Pivalic acidHCID 11430Potassium CarbonateHCID 11371790Bis(adamantan-1-yl)(butyl)phosphaneHCID 866807956-bromo-4-methyl-N-[4-(trifluoromethyl)pyridine-2-yl]pyridine-2-amineHCID 86715345Tert-butyl 3-[1-hydroxy-1-(1,3-thiazol-2-yl)ethyl]pyrrolidine-1-carboxylate

生成物 1

HCID 86715346
Tert-butyl 3-{1-hydroxy-1-[5-(4-methyl-6-{[4-(trifluoromethyl)-pyridin-2-yl]amino}pyridin-2-yl)-1,3-thiazol-2-yl]ethyl}pyrrolidine-1-carboxylate

試薬・触媒・溶媒 2

HCID 9811564Bis(dibenzylideneacetone)palladium触媒HCID 31374Dimethylacetamide溶媒

反応条件

温度
130 °C

実験手順

tert-Butyl 3-[1-hydroxy-1-(1,3-thiazol-2-yl)ethyl]pyrrolidine-1-carboxylate (100 mg, 0.335 mmol), 6-bromo-4-methyl-N-[4-(trifluoromethyl)pyridin-2-yl]pyridin-2-amine (112 mg, 0.337 mmol), butyl di-1-adamantylphosphine (25 mg, 0.070 mmol), tris(dibenzylideneacetone)dipalladium(0) (16.3 mg, 0.018 mmol), pivalic acid (0.018 mL, 0.157 mmol), potassium carbonate (140 mg, 1.013 mmol) and N,N-dimethylacetamide (1 mL) were combined and the mixture was evacuated and purged with nitrogen 3 times then heated to 130° C. for 7 hours. The mixture was filtered then extracted with ethyl acetate. The organic phase was washed with water and brine, dried over sodium sulfate, and concentrated under reduced pressure to afford tert-butyl 3-{1-hydroxy-1-[5-(4-methyl-6-{[4-(trifluoromethyl)-pyridin-2-yl]amino}pyridin-2-yl)-1,3-thiazol-2-yl]ethyl}pyrrolidine-1-carboxylate, which was used in a subsequent step without further purification. MS ESI calc'd. for C26H30F3N5O3S [M+H]+ 550. found 550.

後処理

  1. customthe mixture was evacuated
  2. custompurged with nitrogen 3 times
  3. filtrationThe mixture was filtered
  4. extractionthen extracted with ethyl acetate
  5. washThe organic phase was washed with water and brine
  6. dry with materialdried over sodium sulfate
  7. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-efdfb72df5384e3e96522f795d33ca09
出典データセット
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09120785B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート