Acetic Acid → HCID 20184537、化合物

HRID 2309909ノート

反応式

HRID 2309909 の反応式
[NH2:1][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.[O-:24][C:25]#[N:26].[K+].C(O)(=O)C>O1CCCC1>[NH2:26][C:25]([NH:1][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)=[O:24]

参加物

5

反応物 3

HCID 176Acetic AcidHCID 11378442Potassium cyanateHCID 20184521HCID 20184521、化合物

生成物 1

HCID 20184537HCID 20184537、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

One gram (3.0 mmol) of 5-amino-2-(2'-methoxy-4'-methanesulfonyloxy-phenyl)-benzimidazole were dissolved in 20 ml of pure tetrahydrofuran, and then 2.0 gm of potassium cyanate and 5 ml of 2M acetic acid were added successively. After the mixture refluxed for eight hours, the solvent was evaporated off in vacuo, and the residue was mixed with 10 ml of water and neutralized with 5% sodium bicarbonate solution. The crude product precipitated was subjected to suction filtration and chromatographed over 200 gm of silica gel (eluant: methylene chloride with 8% ethanol).

後処理

  1. temperatureAfter the mixture refluxed for eight hours
  2. customthe solvent was evaporated off in vacuo
  3. additionthe residue was mixed with 10 ml of water and neutralized with 5% sodium bicarbonate solution
  4. customThe crude product precipitated
  5. filtrationwas subjected to suction filtration
  6. customchromatographed over 200 gm of silica gel (eluant: methylene chloride with 8% ethanol)

出典と根拠

ORDレコード
ord-fb3d288f7a7e480cafcec2d2e385f9ea
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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