Ammonia → HCID 20184552, 화합물

HRID 2309907노트

반응식

HRID 2309907 반응식
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

참가 물질

6

반응물 3

HCID 222AmmoniaHCID 20184521HCID 20184521, 화합물HCID 23668193Sodium Nitrite

생성물 1

HCID 20184552HCID 20184552, 화합물

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 962Water용매2회

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-e4646a5dfaa24a84839f13b93ac13ab1
출처 데이터셋
uspto-grants-1987_09
특허 번호
US04696931

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