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Water → 9-(2-Chloroethyl)-9H-carbazole

HRID 1860349
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HRID 1860349 반응식
[CH:1]1[C:13]2[NH:12][C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5]=2[CH:4]=[CH:3][CH:2]=1.[Cl:14][CH2:15][CH2:16]OS(C1C=CC(C)=CC=1)(=O)=O.[OH-].[Na+].O>CC(C)=O>[Cl:14][CH2:15][CH2:16][N:12]1[C:11]2[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=2[C:5]2[C:13]1=[CH:1][CH:2]=[CH:3][CH:4]=2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 6639Ethanol, 2-chloro-, 1-(4-methylbenzenesulfonate)HCID 6854CarbazoleHCID 14798Sodium Hydroxide

생성물 1

HCID 143539-(2-Chloroethyl)-9H-carbazole수율 43.2%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

17.9 g (107 mmol) of carbazole and 500 ml of acetone as solvent were placed in a 1000 ml four-necked flask with a mechanical stirrer and bulb-shaped cooler. To this was added an aqueous solution prepared from 22.0 g (93.7 mmol)of 2-chloroethyl-p-toluene sulfonate, 12.5 g of sodium hydroxide and 9.2 ml of water. The resultant product was heated to 60° C. in a silicone oil bath, and subjected to the reaction for 20 hours. After the reaction was completed, the product was cooled to the ambient temperature. The precipitated solid was subjected to suction filtration with a glass filter. The resultant liquid was concentrated in an evaporator and dried under vacuum to obtain a brown solid, which was recrystallized in the presence of ligroin to obtain 9.3 g of a white crystal.

후처리

  1. additionTo this was added an aqueous solution
  2. customsubjected to the reaction for 20 hours
  3. filtrationThe precipitated solid was subjected to suction filtration with a glass
  4. filtrationfilter
  5. concentrationThe resultant liquid was concentrated in an evaporator
  6. customdried under vacuum
  7. customto obtain a brown solid, which
  8. customwas recrystallized in the presence of ligroin

출처 및 근거

ORD 기록
ord-443f5ab4f0a64558aabceff952a781e8
출처 데이터셋
uspto-grants-2003_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06528657B2

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