Sodium Bicarbonate → HCID 49821534, 화합물

HRID 74317노트

반응식

HRID 74317 반응식
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[O:9][C:8]([C:10]3[CH:11]=[CH:12][C:13]([NH:17][CH2:18][CH2:19][CH3:20])=[C:14]([CH:16]=3)[NH2:15])=[N:7][C:6]=2[CH:21]=1.Cl.[C:23](=N)(OC)[CH3:24].C(=O)([O-])O.[Na+]>C(O)C>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[O:9][C:8]([C:10]3[CH:11]=[CH:12][C:13]4[N:17]([CH2:18][CH2:19][CH3:20])[C:23]([CH3:24])=[N:15][C:14]=4[CH:16]=3)=[N:7][C:6]=2[CH:21]=1

참가 물질

5

반응물 3

HCID 516892Sodium BicarbonateHCID 10313100Ethanimidic acid, methyl ester, hydrochloride (1:1)HCID 674986575-(5-Chlorobenzoxazol-2-yl)-2-n-propylaminoaniline

생성물 1

HCID 49821534HCID 49821534, 화합물수율 72%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a solution of 5-(5-chlorobenzoxazol-2-yl)-2-n-propylaminoaniline (see Working Example 135-1) (200 mg, 0.663 mmol) in ethanol (5 mL) was added methyl acetimidate hydrochloride (123 mg, 0.995 mmol), and this was heated to reflux for 5 hours. After the reaction was complete, saturated aqueous sodium hydrogen carbonate solution was added, and this was extracted with chloroform. The organic layer obtained was dried over anhydrous sodium sulfate, filtered, and concentrated to give crude crystals that were washed with diethyl ether to yield the title compound (155 mg, 72% yield) as green crystals.

후처리

  1. temperaturethis was heated
  2. temperatureto reflux for 5 hours
  3. extractionthis was extracted with chloroform
  4. customThe organic layer obtained
  5. dry with materialwas dried over anhydrous sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customto give crude crystals that
  9. washwere washed with diethyl ether

출처 및 근거

ORD 기록
ord-dcc6e37fba5a420b9ecf5315a63b1015
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08829035B2

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