Triethylamine → HCID 19108707、化合物

HRID 1493978

反応式

HRID 1493978 の反応式
[S:1](Cl)(=[O:4])(=[O:3])[NH2:2].[Cl:6][C:7]1[CH:16]=[CH:15][CH:14]=[CH:13][C:8]=1[O:9][CH2:10][CH2:11][OH:12].C(N(CC)CC)C>C(#N)C>[Cl:6][C:7]1[CH:16]=[CH:15][CH:14]=[CH:13][C:8]=1[O:9][CH2:10][CH2:11][O:12][S:1](=[O:4])(=[O:3])[NH2:2]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 24499Chlorosulfamic acidHCID 849332-(2-Chlorophenoxy)ethanol

生成物 1

HCID 19108707HCID 19108707、化合物収率 58%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

The title compound was obtained using the following procedure: The sulfamoyl chloride solution prepared in (a) was reacted as in Example 4 with 17.3 g (0.100 mole) of 2-(2-chlorophenoxy)ethanol and 40.4 g (0.400 mole) of triethylamine in 100 ml of acetonitrile followed by extraction, washing and concentration procedures of Example 4 through the first evaporation. The viscous, oily residue was partitioned between 500 ml of water and 500 ml of ethyl ether. The organic layer was washed with four 300 ml portions of water (pH of wash finally neutral to pH paper), dried over magnesium sulfate and the solvent evaporated under reduced pressure to give a white solid. The solid was recrystallized from ethyl ether-petroleum ether (bp 30°-60° C.) to give 14.5 g (58%) of title compound as white solid, mp 84.5°-86° C.

後処理

  1. extractionfollowed by extraction
  2. washwashing
  3. concentrationconcentration procedures of Example 4
  4. customthrough the first evaporation
  5. customThe viscous, oily residue was partitioned between 500 ml of water and 500 ml of ethyl ether
  6. washThe organic layer was washed with four 300 ml portions of water (pH
  7. washof wash finally neutral to pH paper),
  8. dry with materialdried over magnesium sulfate
  9. customthe solvent evaporated under reduced pressure
  10. customto give a white solid
  11. customThe solid was recrystallized from ethyl ether-petroleum ether (bp 30°-60° C.)

出典と根拠

ORDレコード
ord-1fccb8bc43b44448a43a5370cffb4272
出典データセット
uspto-grants-1991_06
特許番号
US05025031

関連ノート

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