Dihexylamine → 4-(N,N-di-n-hexylamino)-3-ethoxy-1,1-dioxo-1,2,5-thiadiazole

HRID 495039

反応式

HRID 495039 の反応式
[CH2:1]([NH:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH3:13])[CH2:2][CH2:3][CH2:4][CH2:5][CH3:6].[CH2:14]([O:16][C:17]1[C:21](OCC)=[N:20][S:19](=[O:26])(=[O:25])[N:18]=1)[CH3:15]>C(O)C>[CH2:8]([N:7]([C:21]1[C:17]([O:16][CH2:14][CH3:15])=[N:18][S:19](=[O:26])(=[O:25])[N:20]=1)[CH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH3:6])[CH2:9][CH2:10][CH2:11][CH2:12][CH3:13]

参加物

4

反応物 2

HCID 8920DihexylamineHCID 112179953,4-Diethoxy-1,2,5-thiadiazole-1,1-dioxide

生成物 1

HCID 221387874-(N,N-di-n-hexylamino)-3-ethoxy-1,1-dioxo-1,2,5-thiadiazole収率 72.4%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Dihexylamine (90 mg, 0.48 mmol) was added to a solution of 3,4-diethyloxy-1,1-dioxo-1,2,5-thiadiazole (100 mg, 0.48 mmol) in ethanol (5 mL) and the reaction stirred overnight at room temperature. The solvent was removed under reduced pressure and the residue absorbed onto silica gel, and purified by flash column chromatography (silica, hexane:EtOAc 3:1) to yield 4-(N,N-di-n-hexylamino)-3-ethoxy-1,1-dioxo-1,2,5-thiadiazole (120 mg, 72%). MS (EI, m/e 345).

後処理

  1. customThe solvent was removed under reduced pressure
  2. customthe residue absorbed onto silica gel
  3. custompurified by flash column chromatography (silica, hexane:EtOAc 3:1)

出典と根拠

ORDレコード
ord-9e67ebadc2a440d98db9cb0fd6976dbc
出典データセット
uspto-grants-2009_05
特許番号
US07538215B2

関連ノート

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