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4-Methylmorpholine → 8-[3-(Acetylsarcosylamino)-2,6-dichlorobenzyloxy]-2-methylimidazo[1,2-a]pyridine

HRID 1290163
ノート
印刷プレビュー

反応式

HRID 1290163 の反応式
C(Cl)(=O)C(C)(C)C.[C:8]([N:11]([CH2:13][C:14]([OH:16])=O)[CH3:12])(=[O:10])[CH3:9].CN1CCOCC1.[NH2:24][C:25]1[C:26]([Cl:44])=[C:27]([C:40]([Cl:43])=[CH:41][CH:42]=1)[CH2:28][O:29][C:30]1[C:31]2[N:32]([CH:36]=[C:37]([CH3:39])[N:38]=2)[CH:33]=[CH:34][CH:35]=1>CN1CCCC1=O>[C:8]([N:11]([CH2:13][C:14]([NH:24][C:25]1[C:26]([Cl:44])=[C:27]([C:40]([Cl:43])=[CH:41][CH:42]=1)[CH2:28][O:29][C:30]1[C:31]2[N:32]([CH:36]=[C:37]([CH3:39])[N:38]=2)[CH:33]=[CH:34][CH:35]=1)=[O:16])[CH3:12])(=[O:10])[CH3:9]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 79724-MethylmorpholineHCID 62493Pivaloyl chlorideHCID 10975514N-Acetyl-N-methylglycineHCID 189235318-[3-Amino-2,6-dichlorobenzyloxy]-2-methylimidazo[1,2-a]pyridine

生成物 1

HCID 189232858-[3-(Acetylsarcosylamino)-2,6-dichlorobenzyloxy]-2-methylimidazo[1,2-a]pyridine収率 38.5%

試薬・触媒・溶媒 1

HCID 13387
N-methyl-2-pyrrolidone
溶媒

実験手順

Pivaloyl chloride (0.22 ml) was added dropwise to a mixture of acetylsarcosine (264 mg), N-methylmorpholine (0.22 ml) and N-methylpyrrolidone (30 ml) under a dry ice-tetrachloromethane bath cooling. This mixture was stirred for 10 minutes under ice-cooling, and 8-[3-amino-2,6-dichlorobenzyloxy]-2-methylimidazo[1,2-a]pyridine (500 mg) was added thereto under a dry ice-tetrachloromethane bath cooling. The mixture was stirred for 22 hours at ambient temperature. The mixture was partitioned between ethyl acetate and a saturated aqueous sodium bicarbonate solution, and the aqueous layer was extracted with ethyl acetate twice. The combined organic layer was dried over magnesium sulfate and concentrated in vacuo, and the residue was purified by flash column chromatography (methylene chloride:methanol=50:1, V/V) to give 8-[3-(acetylsarcosylamino)-2,6-dichlorobenzyloxy]-2-methylimidazo[1,2-a]pyridine (260 mg).

後処理

  1. temperaturecooling
  2. temperaturecooling
  3. temperatureunder a dry ice-tetrachloromethane bath cooling
  4. stirringThe mixture was stirred for 22 hours at ambient temperature
  5. customThe mixture was partitioned between ethyl acetate
  6. extractiona saturated aqueous sodium bicarbonate solution, and the aqueous layer was extracted with ethyl acetate twice
  7. dry with materialThe combined organic layer was dried over magnesium sulfate
  8. concentrationconcentrated in vacuo
  9. customthe residue was purified by flash column chromatography (methylene chloride:methanol=50:1, V/V)

出典と根拠

ORDレコード
ord-2867559b429546d288d5954799d917ae
出典データセット
uspto-grants-1998_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05750699

反応ノート

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