ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Methanol → HCID 59627738、化合物

HRID 1930105
ノート
印刷プレビュー

反応式

HRID 1930105 の反応式
Cl[C:2]1[N:7]=[C:6]([C:8]([NH2:10])=[O:9])[C:5]([CH3:11])=[N:4][C:3]=1[CH3:12].[Cl:13][C:14]1[CH:19]=[C:18]([CH2:20][C:21]([O:23][CH3:24])=[O:22])[CH:17]=[CH:16][C:15]=1[C:25]1[C:30]([F:31])=[CH:29][C:28](B2OC(C)(C)C(C)(C)O2)=[CH:27][C:26]=1[F:41].P([O-])([O-])([O-])=O.[K+].[K+].[K+].CO>COCCOC.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.Cl[Pd]Cl.[Fe+2].C(Cl)Cl.O>[C:8]([C:6]1[N:7]=[C:2]([C:28]2[CH:27]=[C:26]([F:41])[C:25]([C:15]3[CH:16]=[CH:17][C:18]([CH2:20][C:21]([O:23][CH3:24])=[O:22])=[CH:19][C:14]=3[Cl:13])=[C:30]([F:31])[CH:29]=2)[C:3]([CH3:12])=[N:4][C:5]=1[CH3:11])(=[O:9])[NH2:10]
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 4

HCID 887MethanolHCID 62657Potassium Phosphate, TribasicHCID 579920346-Chloro-3,5-dimethylpyrazine-2-carboxamide2 回HCID 59627631HCID 59627631、化合物2 回

生成物 1

HCID 59627738HCID 59627738、化合物収率 53.8%

試薬・触媒・溶媒 3

HCID 178418807
HCID 178418807、化合物
触媒
HCID 962Water溶媒
HCID 80711,2-Dimethoxyethane溶媒

反応条件

温度
80 °C

実験手順

A solution of 6-chloro-3,5-dimethylpyrazine-2-carboxamide (Intermediate A) (228 mg, 1.23 mmol) and methyl 2-(2-chloro-2′,6′-difluoro-4′-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)biphenyl-4-yl)acetate (Intermediate 2-2; 521 mg, 1.23 mmol) and potassium phosphate, tri-basic (314 mg, 1.48 mmol) in DME (15 mL), MeOH (3.75 mL) and water (3.75 mL) was thoughroughly degassed. The mixture was treated with PdCl2(dppf)-DCM adduct (50.3 mg, 0.06 mmol), degassed again and the atmosphere replaced with nitrogen before being heated to 80° C. for 17 hours. The reaction mixture was allowed to cool to room temperature and then evaporated. The crude product was partitioned between EtOAc (75 mL), and 2M HCl (50 mL), the aqueous phase was extracted with a further 80 mL of EtOAc. The organic extracts were combined, dried over MgSO4, filtered and evaporated to afford crude product. The crude product was purified by flash silica chromatography, elution gradient 10 to 70% EtOAc in isohexane. Pure fractions were evaporated to dryness to afford methyl 2-(4′-(6-carbamoyl-3,5-dimethylpyrazin-2-yl)-2-chloro-2′,6′-difluorobiphenyl-4-yl)acetate (295 mg, 53.7%) as a white solid.

後処理

  1. customdegassed again
  2. temperatureto cool to room temperature
  3. customevaporated
  4. customThe crude product was partitioned between EtOAc (75 mL), and 2M HCl (50 mL)
  5. extractionthe aqueous phase was extracted with a further 80 mL of EtOAc
  6. dry with materialdried over MgSO4
  7. filtrationfiltered
  8. customevaporated
  9. customto afford crude product
  10. customThe crude product was purified by flash silica chromatography, elution gradient 10 to 70% EtOAc in isohexane
  11. customPure fractions were evaporated to dryness

出典と根拠

ORDレコード
ord-5130ac02f1204963946ec9218d1679dc
出典データセット
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08188092B2

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