Dichloromethane → 4-(7-Chloro-4-quinazolinylamino)-N-(2-diethylaminoethyl) benzenesulphonamide

HRID 235650노트

반응식

HRID 235650 반응식
Cl.[Cl:2][C:3]1[CH:12]=[C:11]2[C:6]([C:7]([NH:13][C:14]3[CH:19]=[CH:18][C:17]([S:20](Cl)(=[O:22])=[O:21])=[CH:16][CH:15]=3)=[N:8][CH:9]=[N:10]2)=[CH:5][CH:4]=1.Cl.S(Cl)(Cl)(=O)=O.C(Cl)Cl.[CH2:33]([N:35]([CH2:39][CH3:40])[CH2:36][CH2:37][NH2:38])[CH3:34]>O>[Cl:2][C:3]1[CH:12]=[C:11]2[C:6]([C:7]([NH:13][C:14]3[CH:19]=[CH:18][C:17]([S:20]([NH:38][CH2:37][CH2:36][N:35]([CH2:39][CH3:40])[CH2:33][CH3:34])(=[O:22])=[O:21])=[CH:16][CH:15]=3)=[N:8][CH:9]=[N:10]2)=[CH:5][CH:4]=1

참가 물질

6

반응물 4

HCID 6344DichloromethaneHCID 60993N,N-DiethylethylenediamineHCID 19012189Sulphonylchloride hydrochlorideHCID 212739544-(7-Chloro-4-quinazolinylamino)benzenesulphonyl chloride hydrochloride

생성물 1

HCID 135372024-(7-Chloro-4-quinazolinylamino)-N-(2-diethylaminoethyl) benzenesulphonamide

시약·촉매·용매 1

HCID 962Water용매

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온도
10 °C

실험 절차

4-(7-Chloro-4-quinazolinylamino)benzenesulphonyl chloride hydrochloride (36.0 g obtainable from the title compound of Example 1) and methylene chloride (180 ml) were cooled under nitrogen to 5° C. N,N-Diethylethylenediamine (35.4 g) was then added at 5°-10° C. over 20 minutes to give a light yellow solution. The solution was stirred for 2 hours under nitrogen at 5° to 15° C. and then water (200 ml) was added. A white solid precipitated. The mixture was cooled to 10° C. and the solid was filtered off, washed with water (2×40 ml) and with chloroform (2×40 ml) and dried in an oven to give 279 g of title compound.

후처리

  1. customto give a light yellow solution
  2. customA white solid precipitated
  3. filtrationthe solid was filtered off
  4. washwashed with water (2×40 ml) and with chloroform (2×40 ml)
  5. customdried in an oven

출처 및 근거

ORD 기록
ord-8665aaec3b5e4843bf2169866c7a0ac4
출처 데이터셋
uspto-grants-1987_02
특허 번호
US04640920

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