Methanol → HCID 67497701, 화합물

HRID 74268노트

반응식

HRID 74268 반응식
CO.[CH:3]1([NH:13][C:14]2[CH:20]=[CH:19][C:18]([C:21]3[O:22][C:23]4[CH:29]=[CH:28][CH:27]=[CH:26][C:24]=4[N:25]=3)=[CH:17][C:15]=2[NH2:16])[C:12]2[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=2)[CH2:6][CH2:5][CH2:4]1.Cl.[C:31](=N)(OC)[CH3:32]>O>[O:22]1[C:23]2[CH:29]=[CH:28][CH:27]=[CH:26][C:24]=2[N:25]=[C:21]1[C:18]1[CH:19]=[CH:20][C:14]2[N:13]([CH:3]3[C:12]4[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=4)[CH2:6][CH2:5][CH2:4]3)[C:31]([CH3:32])=[N:16][C:15]=2[CH:17]=1

참가 물질

5

반응물 3

HCID 887MethanolHCID 10313100Ethanimidic acid, methyl ester, hydrochloride (1:1)HCID 674979522-(2-(1,2,3,4-Tetrahydronaphthalen-1-yl)aminoanilin-5-yl)benzoxazole

생성물 1

HCID 67497701HCID 67497701, 화합물수율 49.4%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a methanol (5 mL) solution of 2-(2-(1,2,3,4-tetrahydronaphthalen-1-yl)aminoanilin-5-yl)benzoxazole (see Working Example 87-1) (0.30 g, 0.8 mmol) was added methyl acetimidate hydrochloride (0.10 g, 0.9 mmol), and this was heated to reflux for 3 hours. After the reaction solution was cooled, water 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 residue obtained was purified by silica gel column chromatography to yield the title compound (0.15 g, 47% yield) as a colorless amorphous mass.

후처리

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

출처 및 근거

ORD 기록
ord-7c8af375083148a3996f5290d4cb4ece
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08829035B2

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