Ammonia → HCID 20184552、化合物

HRID 2309907ノート

反応式

HRID 2309907 の反応式
N[C:2]1[CH:23]=[CH:22][C:5]2[N:6]=[C:7]([C:9]3[CH:14]=[CH:13][C:12]([O:15][S:16]([CH3:19])(=[O:18])=[O:17])=[CH:11][C:10]=3[O:20][CH3:21])[NH:8][C:4]=2[CH:3]=1.N([O-])=[O:25].[Na+].N>C(O)(=O)C.O>[OH:25][C:2]1[CH:23]=[CH:22][C:5]2[N:6]=[C:7]([C:9]3[CH:14]=[CH:13][C:12]([O:15][S:16]([CH3:19])(=[O:17])=[O:18])=[CH:11][C:10]=3[O:20][CH3:21])[NH:8][C:4]=2[CH:3]=1

参加物

6

反応物 3

HCID 222AmmoniaHCID 20184521HCID 20184521、化合物HCID 23668193Sodium Nitrite

生成物 1

HCID 20184552HCID 20184552、化合物

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 962Water溶媒2 回

実験手順

An amount of 3.2 (9.6 mmol) of 5-amino-2-(2'-methoxy-4'-methanesulfonyloxy-phenyl)-benzimidazole was dissolved in 509 ml of glacial acetic acid, and then a solution of 1.38 gm (20 mmol) of sodium nitrite in 5.0 ml of water was added dropwise, under stirring. After one hour, the mixture was diluted with 100 ml of water, and the solution was refluxed for 1.5 hours. Subsequent to cooling, the solution was adjusted to a pH of 5 with concentrated ammonia and extracted three times, each time with 40 ml of methyl ethyl ketone, and the extracts are dried and concentrated by evaporation in vacuo. The oily residue was chromatographed over 500 gm of aluminium oxide (neutral) (eluant: methylene chloride with 8% ethanol).

後処理

  1. temperaturethe solution was refluxed for 1.5 hours
  2. temperatureSubsequent to cooling
  3. extractionextracted three times
  4. dry with materialeach time with 40 ml of methyl ethyl ketone, and the extracts are dried
  5. concentrationconcentrated by evaporation in vacuo
  6. customThe oily residue was chromatographed over 500 gm of aluminium oxide (neutral) (eluant: methylene chloride with 8% ethanol)

出典と根拠

ORDレコード
ord-e4646a5dfaa24a84839f13b93ac13ab1
出典データセット
uspto-grants-1987_09
特許番号
US04696931

反応ノート

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