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Pivalic acid → HCID 178439376、化合物

HRID 81240
ノート
印刷プレビュー

反応式

HRID 81240 の反応式
C12(P(C34CC5CC(CC(C5)C3)C4)CCCC)CC3CC(CC(C3)C1)C2.[Cl:26][C:27]1[CH:28]=[C:29]([C:33]2[C:38]3[N:39]([CH2:42][C@H:43]4[CH2:48][CH2:47][C@H:46]([CH3:49])[CH2:45][CH2:44]4)[CH:40]=[N:41][C:37]=3[CH:36]=[C:35]([C:50]#[N:51])[N:34]=2)[CH:30]=[N:31][CH:32]=1.Br[C:53]1[CH:58]=[C:57]([CH:59]([CH3:61])[CH3:60])[CH:56]=[CH:55][N:54]=1.[F-].[Cs+].C(O)(=O)C(C)(C)C>C([O-])(=O)C.[Pd+2].C([O-])(=O)C.O1CCOCC1>[Cl:26][C:27]1[CH:28]=[C:29]([C:33]2[C:38]3[N:39]([CH2:42][C@H:43]4[CH2:48][CH2:47][C@H:46]([CH3:49])[CH2:45][CH2:44]4)[C:40]([C:53]4[CH:58]=[C:57]([CH:59]([CH3:61])[CH3:60])[CH:56]=[CH:55][N:54]=4)=[N:41][C:37]=3[CH:36]=[C:35]([C:50]#[N:51])[N:34]=2)[CH:30]=[N:31][CH:32]=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

8

反応物 5

HCID 6417Pivalic acidHCID 25953Cesium fluorideHCID 11371790Bis(adamantan-1-yl)(butyl)phosphaneHCID 457879862-Bromo-4-isopropylpyridineHCID 178461253HCID 178461253、化合物

生成物 1

HCID 178439376HCID 178439376、化合物

試薬・触媒・溶媒 2

HCID 167845palladium(II) acetate触媒
HCID 312751,4-Dioxane溶媒

反応条件

温度
50 °C

実験手順

A vial equipped with a stir bar was charged with di(1-adamantyl)-n-butylphosphine (cataCXium A, Strem) (143.2 mg, 0.40 mmol) and palladium acetate (45 mg, 0.20 mmol). Dioxane (2.5 mL) was added, and the mixture was degassed with N2. The vial was then sealed and heated at 50° C. for 30 minutes. The catalyst slurry was then cooled back to room temperature, and 1.5 mL of this catalyst slurry was added via syringe to a second vial equipped with a stir bar and containing 4-(5-chloropyridin-3-yl)-3-[(trans-4-methylcyclohexyl)methyl]-3H-imidazo[4,5-c]pyridine-6-carbonitrile (Preparative Example 3.1, Step 2;100 mg, 0.273 mmol), 2-bromo-4-isopropylpyridine (109 mg, 0.547 mmol; purchased from Combiphos), cesium fluoride (125 mg, 0.82 mmol), and pivalic acid (36.3 mg, 0.355 mmol). The reaction was degassed with N2 for 2 minutes, and then the vial was sealed and heated at 110° C. for 20 hours. The reaction was then cooled to room temperature, diluted with hexanes (2 mL) and CH2Cl2 (2 mL), and loaded directly onto a silica gel column. Purification with 0 to 75% EtOAc/hexanes afforded 4-(5-chloropyridin-3-yl)-3-[(trans-4-methylcyclohexyl)methyl]-2-[4-(propan-2-yl)pyridin-2-yl]-3H-imidazo[4,5-c]pyridine-6-carbonitrile. MS ESI calc'd for C28H29ClN6 [M+H]+=485. found=485.

後処理

  1. customA vial equipped with a stir bar
  2. customthe mixture was degassed with N2
  3. customThe vial was then sealed
  4. temperatureThe catalyst slurry was then cooled back to room temperature
  5. addition1.5 mL of this catalyst slurry was added via syringe to a second
  6. customvial equipped with a stir bar
  7. customThe reaction was degassed with N2 for 2 minutes
  8. customthe vial was sealed
  9. temperatureheated at 110° C. for 20 hours
  10. temperatureThe reaction was then cooled to room temperature
  11. additiondiluted with hexanes (2 mL) and CH2Cl2 (2 mL)
  12. customPurification with 0 to 75% EtOAc/hexanes

出典と根拠

ORDレコード
ord-a9812673d4c24bb4ac6c8d34feb97f52
出典データセット
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08846657B2

反応ノート

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