Acetic Acid → HCID 20184537, 화합물

HRID 1380765노트

반응식

HRID 1380765 반응식
[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]

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 11378442Potassium cyanateHCID 20184521HCID 20184521, 화합물

생성물 1

HCID 20184537HCID 20184537, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-a7e7c6ee94a94560bceee761005ddb98
출처 데이터셋
uspto-grants-1986_04
특허 번호
US04582837

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