1,2-Dibromoethane → HCID 22646390、化合物

HRID 393519

反応式

HRID 393519 の反応式
O[C:2]1[C:14]2[C:13]3[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=3)[NH:7][C:6]=2[CH:5]=[CH:4][CH:3]=1.[Br:15][CH2:16][CH2:17]Br.[OH-:19].[Na+]>O>[Br:15][CH2:16][CH2:17][O:19][C:3]1[CH:4]=[CH:5][C:6]2[NH:7][C:8]3[C:13]([C:14]=2[CH:2]=1)=[CH:12][CH:11]=[CH:10][CH:9]=3

参加物

5

反応物 3

HCID 78391,2-DibromoethaneHCID 14798Sodium HydroxideHCID 1042514-Hydroxycarbazole

生成物 1

HCID 22646390HCID 22646390、化合物収率 32%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 1.83 g (10 mmol) of 4-hydroxycarbazole (J. Chem. Soc. (1955), 3475-3477; J. Med. Chem. (1964) 7, 158-161), 1.08 ml (12,5 mmol) of 1,2-dibromoethane and 2.6 ml (10.5 mmol) of a 4 M aqueous solution of NaOH in 2 ml of water is heated under reflux for 5 hours. After the temperature returns to 20° C., the product is extracted using 2 times 30 ml of CH2Cl2. The organic solutions collected are then successively washed with 20 ml of water and 20 ml of salt water. After drying over MgSO4, filtration and concentration under vacuum, the residue is purified on a silica column (eluent: heptane/AcOEt: 80/20). A beige powder is obtained with a yield of 32%. Melting point: 135-136° C.

後処理

  1. temperatureis heated
  2. temperatureunder reflux for 5 hours
  3. extractionAfter the temperature returns to 20° C., the product is extracted
  4. customThe organic solutions collected
  5. washare then successively washed with 20 ml of water and 20 ml of salt water
  6. dry with materialAfter drying over MgSO4, filtration and concentration under vacuum
  7. customthe residue is purified on a silica column (eluent: heptane/AcOEt: 80/20)
  8. customA beige powder is obtained with a yield of 32%

出典と根拠

ORDレコード
ord-311e2387966e4a3692f8657e546c1282
出典データセット
uspto-grants-2004_10
特許番号
US06809090B2

関連ノート

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