Triethylamine → HCID 67266799、化合物

HRID 602775

反応式

HRID 602775 の反応式
[C:1]1([S:7]([CH2:10][C:11]([NH:13][NH2:14])=[O:12])(=[O:9])=[O:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[Cl-].Cl[C:17](=[N+:19]([CH3:21])[CH3:20])Cl.C(N(CC)CC)C>C(Cl)(Cl)Cl>[C:1]1([S:7]([CH2:10][C:11]2[O:12][C:17]([N:19]([CH3:21])[CH3:20])=[N:14][N:13]=2)(=[O:8])=[O:9])[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 2723945Phosgeniminium chlorideHCID 11378890Benzenesulfonyl-acetic acid hydrazide

生成物 1

HCID 67266799HCID 67266799、化合物

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

To 3.0 g (14.0 mmol) of benzenesulfonyl-acetic acid hydrazide in 100 mL of CHCl3, 3.41 g (21.0 mmol, 1.5 eq) of dichloromethylene-dimethyl-ammonium chloride and 3.90 mL (28.0 mmol, 2 eq) of triethyl-amine were added. The solution was stirred at reflux for 1 hour, partitioned between aqueous NaOH 0.5M and EtOAc. The combined organic phases were dried over Na2SO4, filtered, evaporated, and column chromatography on silica gel with CH2Cl2/MeOH 100:1 afforded 0.59 g /15%) of (5-benzenesulfonylmethyl-[1,3,4]oxadiazol-2-yl)-dimethyl-amine as a white solid, MS: 268 (MH+).

後処理

  1. temperatureat reflux for 1 hour
  2. custompartitioned between aqueous NaOH 0.5M and EtOAc
  3. dry with materialThe combined organic phases were dried over Na2SO4
  4. filtrationfiltered
  5. customevaporated

出典と根拠

ORDレコード
ord-85e5685164b74fb99db3ed0d1e40f0fb
出典データセット
uspto-grants-2011_03
特許番号
US07906546B2

関連ノート

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