Dimethylsulphamoyl chloride → HCID 20704038、化合物

HRID 904082ノート

反応式

HRID 904082 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

HCID 20704038HCID 20704038、化合物

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-652893c945fb47a98e2a55df151411d4
出典データセット
uspto-grants-1980_10
特許番号
US04230635

反応ノート

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