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1,2-Dichloroethane → HCID 20147792, 화합물

HRID 1982286
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HRID 1982286 반응식
Cl[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH3:8][N:9]([CH3:29])[C:10]1[CH:15]=[CH:14][C:13]([CH:16]2[C:25]3[C:20](=[CH:21][C:22]([N:26]([CH3:28])[CH3:27])=[CH:23][CH:24]=3)[C:18](=[O:19])[O:17]2)=[CH:12][CH:11]=1.[CH3:30][N:31]1C=CC=[CH:32]1.[Cl-].[Al+3].[Cl-].[Cl-].[CH2:40](Cl)CCl>O>[CH3:40][C:2]1[CH:7]=[C:6]([N:31]([CH3:32])[CH3:30])[CH:5]=[CH:4][C:3]=1[CH:16]([C:25]1[CH:24]=[CH:23][C:22]([N:26]([CH3:28])[CH3:27])=[CH:21][C:20]=1[C:18]([OH:17])=[O:19])[C:13]1[CH:14]=[CH:15][C:10]([N:9]([CH3:29])[CH3:8])=[CH:11][CH:12]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 5

HCID 111,2-DichloroethaneHCID 73041-MethylpyrroleHCID 7964ChlorobenzeneHCID 936931(3H)-Isobenzofuranone, 6-(dimethylamino)-3-[4-(dimethylamino)phenyl]-HCID 6451240Aluminum(III) Chloride

생성물 1

HCID 20147792HCID 20147792, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a stirred mixture of 75.0 ml of monochlorobenzene, 7.4 g of 3-(4-dimethylaminophenyl)-6-dimethylaminophthalide and 2.2 g of N-methylpyrrole maintained at 0°-5° C. by means of an external ice-bath, there was slowly added 6.65 g of anhydrous aluminum chloride. After stirring for approximately three hours, there was slowly added with continued cooling at 0°-5° C., 100 ml of water and 100 ml of ethylene dichloride. The layers were separated and the organic layer extracted with 150 ml of fresh water. The organic layer was then extracted with 100 ml of 3N hydrochloric acid, separated and the pH of this aqueous acid layer adjusted to 4.5 with five percent aqueous sodium hydroxide solution. The green solid which had formed was collected by filtration. After reslurrying in a mixture of acetone and methanol, the solid was filtered and dried to obtain 5.2 g of 2-[α-(4-dimethylaminophenyl)-α-(1-methyl-2-pyrrolyl)]methyl-5-dimethylaminobenzoic acid (Formula III: R=CH3 ; X=H; Y=4-(CH3)2 --NC6H4 ; Z=1-CH3 -2-pyrrolyl).

후처리

  1. temperaturemaintained at 0°-5° C. by means of an external ice-bath
  2. additionthere was slowly added
  3. temperaturewith continued cooling at 0°-5° C.
  4. customThe layers were separated
  5. extractionthe organic layer extracted with 150 ml of fresh water
  6. extractionThe organic layer was then extracted with 100 ml of 3N hydrochloric acid
  7. customseparated
  8. customThe green solid which had formed
  9. filtrationwas collected by filtration
  10. additionAfter reslurrying in a mixture of acetone and methanol
  11. filtrationthe solid was filtered
  12. customdried

출처 및 근거

ORD 기록
ord-2dad97f33d5e44f7ad13aad5b8239a55
출처 데이터셋
uspto-grants-1986_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04595768

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