1,2-Dibromoethane → HCID 22646390, 화합물

HRID 393519

반응식

HRID 393519 반응식
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

참가 물질

5

반응물 3

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

생성물 1

HCID 22646390HCID 22646390, 화합물수율 32%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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%

출처 및 근거

ORD 기록
ord-311e2387966e4a3692f8657e546c1282
출처 데이터셋
uspto-grants-2004_10
특허 번호
US06809090B2

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