Water → HCID 21833753, 화합물

HRID 1741084노트

반응식

HRID 1741084 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].[NH2:7][C:8]1[CH:9]=[CH:10][C:11]2[O:27][CH2:26][CH2:25][C:14]3([CH2:19][CH2:18][N:17]([C:20](OCC)=O)[CH2:16][CH2:15]3)[C:12]=2[CH:13]=1.O.[OH-].[Na+]>C1COCC1>[NH2:7][C:8]1[CH:9]=[CH:10][C:11]2[O:27][CH2:26][CH2:25][C:14]3([CH2:19][CH2:18][N:17]([CH3:20])[CH2:16][CH2:15]3)[C:12]=2[CH:13]=1

참가 물질

6

반응물 4

HCID 962Water2회HCID 14798Sodium HydroxideHCID 21226445Aluminium lithium hydride2회HCID 21833717HCID 21833717, 화합물

생성물 1

HCID 21833753HCID 21833753, 화합물수율 86.1%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매3회

실험 절차

A stirred suspension of lithium aluminium hydride (76 mg, 0.0020 mole) in THF (15 ml) at 0° C. under argon was treated with a solution of 6-amino-2,3-dihydro-1'-ethoxycarbonylspiro[4H-benzopyran-4,4'-piperidine] (D104, 300 mg, 0.0010 mole) in THF (5 ml). The reaction mixture was allowed to warm to room temp. and stir for 1.5 h, then treated with more lithium aluminium hydride (38 mg, 0.0010 mole) suspended in THF (5 ml). The mixture was heated under reflux for 0.75 h, then cooled in an ice bath and treated with water (0.10 ml), 10% NaOH solution (0.10 ml) and water (0.30 ml). The resulting mixture was filtered through kieselguhr and the filtrate concentrated in vacuo to afford the title compound as a yellow oil (200 mg, 84%).

후처리

  1. temperatureto warm to room temp.
  2. temperatureThe mixture was heated
  3. temperatureunder reflux for 0.75 h
  4. temperaturecooled in an ice bath
  5. filtrationThe resulting mixture was filtered through kieselguhr
  6. concentrationthe filtrate concentrated in vacuo

출처 및 근거

ORD 기록
ord-507546fd787f4bf0bc20330d3ecb2948
출처 데이터셋
uspto-grants-1999_10
특허 번호
US05972951

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