Potassium Carbonate → HCID 86657762、化合物

HRID 400724

反応式

HRID 400724 の反応式
[C:1]([C:3]1[CH:12]=[C:11]2[C:6]([CH2:7][CH2:8][NH:9][CH2:10]2)=[CH:5][CH:4]=1)#[N:2].C([O-])([O-])=O.[K+].[K+].Br[CH2:20][C:21]([O:23][C:24]([CH3:27])([CH3:26])[CH3:25])=[O:22]>CC#N>[C:1]([C:3]1[CH:12]=[C:11]2[C:6]([CH2:7][CH2:8][N:9]([CH2:20][C:21]([O:23][C:24]([CH3:27])([CH3:26])[CH3:25])=[O:22])[CH2:10]2)=[CH:5][CH:4]=1)#[N:2]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 79177tert-Butyl bromoacetateHCID 101762437-Cyano-1,2,3,4-tetrahydroisoquinoline

生成物 1

HCID 86657762HCID 86657762、化合物

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

To a suspension of 7-cyano-1,2,3,4-tetrahydroisoquinoline (ABCR, 2 g; 12.64 mmol) and K2CO3 (3.49 g, 25.28 mmol) in CH3CN (40 mL), was added tert-butyl bromoacetate (1.96 mL; 13.27 mmol) and the reaction mixture was stirred at RT for 4 hours. Solvents were removed under vacuum and solid residue was extracted with EtOAc from a saturated aqueous solution of NaHCO3, dried over MgSO4 and evaporated under vacuum to give the title compound a as colorless oil (3.32 g; 96%). 1H NMR (DMSO-d6) δ 7.55 (m, 2H), 7.30 (m, 1H), 3.72 (s, 2H), 3.31 (s, 2H), 2.86-2.79 (m, 4H), 1.49 (s, 9H). LC/MS (Method B): 217.1 (M+1-1)+.

後処理

  1. customSolvents were removed under vacuum and solid residue
  2. extractionwas extracted with EtOAc from a saturated aqueous solution of NaHCO3
  3. dry with materialdried over MgSO4
  4. customevaporated under vacuum

出典と根拠

ORDレコード
ord-acb11978ebbf4ae9bcbde03146ecad2a
出典データセット
uspto-grants-2014_06
特許番号
US08741923B2

関連ノート

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