Water → HCID 21833753、化合物

HRID 617735ノート

反応式

HRID 617735 の反応式
[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

参加物

6

反応物 4

HCID 962Water2 回HCID 14798Sodium HydroxideHCID 21226445Aluminium lithium hydride2 回HCID 21833717HCID 21833717、化合物

生成物 1

HCID 21833753HCID 21833753、化合物収率 86.1%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒3 回

実験手順

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] (D6, 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%).

後処理

  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

出典と根拠

ORDレコード
ord-0659f5f3869f4bea8097fecd3de80b90
出典データセット
uspto-grants-1999_09
特許番号
US05952325

反応ノート

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