Sodium Bicarbonate → HCID 67498029、化合物

HRID 74246

反応式

HRID 74246 の反応式
[CH2:1]([NH:5][C:6]1[CH:12]=[CH:11][C:10]([C:13]2[O:14][C:15]3[CH:21]=[CH:20][CH:19]=[CH:18][C:16]=3[N:17]=2)=[CH:9][C:7]=1[NH2:8])[CH2:2][CH2:3][CH3:4].Cl.[C:23](=N)(OC)[CH3:24].C(=O)([O-])O.[Na+]>CO>[O:14]1[C:15]2[CH:21]=[CH:20][CH:19]=[CH:18][C:16]=2[N:17]=[C:13]1[C:10]1[CH:11]=[CH:12][C:6]2[N:5]([CH2:1][CH2:2][CH2:3][CH3:4])[C:23]([CH3:24])=[N:8][C:7]=2[CH:9]=1

参加物

5

反応物 3

HCID 516892Sodium BicarbonateHCID 10313100Ethanimidic acid, methyl ester, hydrochloride (1:1)HCID 674988512-(2-n-Butylaminoanilin-5-yl)benzoxazole

生成物 1

HCID 67498029HCID 67498029、化合物収率 90%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a methanol (5 mL) solution of 2-(2-n-butylaminoanilin-5-yl)benzoxazole (see Working Example 74-2) (300 mg, 1.07 mmol) was added methyl acetimidate hydrochloride (175 mg, 1.60 mmol), and this was heated to reflux for 3 hours. After the reaction was complete, saturated aqueous sodium hydrogen carbonate solution was added, and this was extracted with chloroform. After the organic layer obtained was dried over anhydrous sodium sulfate, it was filtered and concentrated. The crystals obtained were purified by silica gel column chromatography to yield the title compound (293 mg, 90% yield) as white crystals.

後処理

  1. temperaturethis was heated
  2. temperatureto reflux for 3 hours
  3. extractionthis was extracted with chloroform
  4. customAfter the organic layer obtained
  5. dry with materialwas dried over anhydrous sodium sulfate, it
  6. filtrationwas filtered
  7. concentrationconcentrated
  8. customThe crystals obtained
  9. customwere purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-05e87679402e4f8594f18771b0703655
出典データセット
uspto-grants-2014_09
特許番号
US08829035B2

関連ノート

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