Water → HCID 21412112, 화합물

HRID 2071718

반응식

HRID 2071718 반응식
I[CH2:2][CH2:3][CH2:4][CH:5]1[C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=2[CH:9]=[CH:8][C:7]2[CH:16]=[CH:17][CH:18]=[CH:19][C:6]1=2.CN(C)C=O.[C:25]1(=[O:35])[NH:29][C:28](=[O:30])[C:27]2=[CH:31][CH:32]=[CH:33][CH:34]=[C:26]12.[K].O>C(Cl)(Cl)Cl>[C:25]1(=[O:35])[N:29]([CH2:2][CH2:3][CH2:4][CH:5]2[C:11]3[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=3[CH:9]=[CH:8][C:7]3[CH:16]=[CH:17][CH:18]=[CH:19][C:6]2=3)[C:28](=[O:30])[C:27]2=[CH:31][CH:32]=[CH:33][CH:34]=[C:26]12

참가 물질

6

반응물 4

HCID 962WaterHCID 6228DimethylformamideHCID 233288685-(3-iodopropyl)-5H-dibenzo[a,d]cyclohepteneHCID 24194345Phthalimide potassium salt

생성물 1

HCID 21412112HCID 21412112, 화합물

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

5-(3-Iodopropyl)-5H-dibenzo[a,d]cycloheptene, 1.8 g. (0.005 mole), is dissolved in 10 ml. of dimethylformamide. The solution is stirred while 930 mg. (0.0051 mole) of potassium phthalimide is added. When the addition is complete, the mixture is heated to 85°-90° C. for 40 minutes, then cooled, diluted with chloroform and poured into water. The chloroform layer is separated and the aqueous layer extracted further with chloroform. Evaporation of the chloroform gives the product as an oily crystalline solid. Several recrystallizations from isopropyl alcohol gave product, m.p. 125.5°-131.5° C.

후처리

  1. dissolution(0.005 mole), is dissolved in 10 ml
  2. additionWhen the addition
  3. temperaturethe mixture is heated to 85°-90° C. for 40 minutes
  4. temperaturecooled
  5. customThe chloroform layer is separated
  6. extractionthe aqueous layer extracted further with chloroform
  7. customEvaporation of the chloroform

출처 및 근거

ORD 기록
ord-3b5ba246c5794fba8c53474ff6c17a16
출처 데이터셋
uspto-grants-1977_09
특허 번호
US04048223

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