Dimethylsulphamoyl chloride → HCID 20704038, 화합물

HRID 904082노트

반응식

HRID 904082 반응식
[CH3:1][NH:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]([OH:18])([C:14]([F:17])([F:16])[F:15])[C:10]([F:13])([F:12])[F:11])=[CH:5][CH:4]=1.[CH3:19][N:20]([CH3:25])[S:21](Cl)(=[O:23])=[O:22]>N1C=CC=CC=1>[F:17][C:14]([F:15])([F:16])[C:9]([C:6]1[CH:5]=[CH:4][C:3]([N:2]([CH3:1])[S:21]([N:20]([CH3:25])[CH3:19])(=[O:23])=[O:22])=[CH:8][CH:7]=1)([OH:18])[C:10]([F:12])([F:13])[F:11]

참가 물질

4

반응물 2

HCID 83372Dimethylsulphamoyl chlorideHCID 8050151,1,1,3,3,3-Hexafluoro-2-(4-(methylamino)phenyl)propan-2-OL

생성물 1

HCID 20704038HCID 20704038, 화합물

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

To 5.4 g (20 mmole) N-methyl-4-(hexafluoro-2-hydroxy-2-propyl)aniline in 50 ml pyridine add 4.3 g (30 mmole) dimethylsulfamoyl chloride. Stir 16 hours, pour onto water, acidify and extract with Et2O. Wash with 1N NaOH, acidify the aqueous layer, and extract with Et2O. Dry, concentrate and recrystallize first from CCl4, and then from Et2O-hexane to obtain the product; m.p. 63°-65° C.

후처리

  1. additionpour onto water
  2. extractionextract with Et2O
  3. washWash with 1N NaOH
  4. extractionextract with Et2O
  5. customDry
  6. concentrationconcentrate
  7. customrecrystallize first from CCl4
  8. customfrom Et2O-hexane to obtain the product

출처 및 근거

ORD 기록
ord-652893c945fb47a98e2a55df151411d4
출처 데이터셋
uspto-grants-1980_10
특허 번호
US04230635

반응 노트

불러오는 중…