Stannous chloride dihydrate → HCID 22382615、化合物

HRID 1372437ノート

反応式

HRID 1372437 の反応式
[CH2:1]([O:8][C:9]([N:11]1[C:19]2[C:14](=[CH:15][CH:16]=[C:17]([N+:20]([O-])=O)[CH:18]=2)[CH2:13][CH2:12]1)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.O.O.[Sn](Cl)Cl>C(O)C>[NH2:20][C:17]1[CH:18]=[C:19]2[C:14]([CH2:13][CH2:12][N:11]2[C:9]([O:8][CH2:1][C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=2)=[O:10])=[CH:15][CH:16]=1

参加物

4

反応物 2

HCID 61436Stannous chloride dihydrateHCID 223825671-Benzyloxycarbonyl-2,3-dihydro-6-nitroindole

生成物 1

HCID 22382615HCID 22382615、化合物収率 99%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
70 °C

実験手順

A mixture of 1-benzyloxycarbonyl-2,3-dihydro-6-nitroindole (1.0 g, 3.36 mmol) and tin(II) chloride dihydrate (3.78 g, 16.75 mmol) in ethanol (70 mL) was heated at 70° C., under an atmosphere of nitrogen, for 3 hours. The solution was cooled and the solvent evaporated under reduced pressure to give an off-white solid. The solid was partitioned between water (50 mL) and ethyl actate (100 mL) and the aqueous layer basified (pH 11) with 1M sodium hydroxide solution. The mixture was filtered to remove tin salts and the ethyl acetate was separated, dried (MgSO4) and evaporated under reduced pressure to give the amine as a yellow oil (0.89 g, 99%).

後処理

  1. temperatureThe solution was cooled
  2. customthe solvent evaporated under reduced pressure
  3. customto give an off-white solid
  4. customThe solid was partitioned between water (50 mL) and ethyl actate (100 mL)
  5. filtrationThe mixture was filtered
  6. customto remove tin salts
  7. customthe ethyl acetate was separated
  8. dry with materialdried (MgSO4)
  9. customevaporated under reduced pressure

出典と根拠

ORDレコード
ord-1ccb136593f145dfb1af562f856db190
出典データセット
uspto-grants-2007_01
特許番号
US07157585B2

反応ノート

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