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1,2-Dichloroethane → HCID 20147792、化合物

HRID 1982286
ノート
印刷プレビュー

反応式

HRID 1982286 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

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

生成物 1

HCID 20147792HCID 20147792、化合物

試薬・触媒・溶媒 1

HCID 962
Water
溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-2dad97f33d5e44f7ad13aad5b8239a55
出典データセット
uspto-grants-1986_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04595768

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート