1-Bromo-3-chloropropane → HCID 10083926、化合物

HRID 234673

反応式

HRID 234673 の反応式
[CH:1]1[C:14]2[NH:13][C:12]3[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=3)[O:6][C:5]=2[CH:4]=[CH:3][CH:2]=1.[H-].[Na+].Br[CH2:18][CH2:19][CH2:20][Cl:21].[Cl-].[NH4+]>CN(C)C=O>[Cl:21][CH2:20][CH2:19][CH2:18][N:13]1[C:14]2[CH:1]=[CH:2][CH:3]=[CH:4][C:5]=2[O:6][C:7]2[C:12]1=[CH:11][CH:10]=[CH:9][CH:8]=2

参加物

6

反応物 4

HCID 80061-Bromo-3-chloropropaneHCID 24758Sodium hydrideHCID 25517Ammonium ChlorideHCID 67278Phenoxazine

生成物 1

HCID 10083926HCID 10083926、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of phenoxazine (3.7 g, 0.02 mol) in dry dimethylformamide (100 ml) kept under an atmosphere of nitrogen, sodium hydride (1.2 g, 0.03 mol, 60% dispersion in oil) was carefully added. The reaction mixture was left stirring for 15 minutes. 1-Bromo-3-chloro-propane (8.0 g, 0.05 mol) was added and the mixture was left stirring overnight. Ammonium chloride (2.0 g, 0.04 mol) was added, and after continued stirring for 30 minutes, the solution was poured onto water (300 ml). The mixture was extracted with dichloromethane (2×200 ml). The combined organic extracts were dried (MgSO4), filtered and the solvent evaporated in vacuo. 10-(3-Chloropropyl)-10H-phenoxazine was obtained in quantitative yield as an oil and used without further purification. Rf : 0.68 (SiO2 ; n-heptane/ethyl acetate=1:1).

後処理

  1. waitThe reaction mixture was left
  2. waitthe mixture was left
  3. stirringstirring overnight
  4. stirringafter continued stirring for 30 minutes
  5. additionthe solution was poured onto water (300 ml)
  6. extractionThe mixture was extracted with dichloromethane (2×200 ml)
  7. dry with materialThe combined organic extracts were dried (MgSO4)
  8. filtrationfiltered
  9. customthe solvent evaporated in vacuo

出典と根拠

ORDレコード
ord-4c05083943d447c6937510d953c2564d
出典データセット
uspto-grants-1997_01
特許番号
US05595989

関連ノート

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