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Sec-Butylamine → HCID 12764046, 화합물

HRID 1903751
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HRID 1903751 반응식
[C:1]([C:3]1[CH:13]=[C:12]([NH:14][C:15](=[O:21])[CH2:16][CH2:17][CH2:18][CH2:19][CH3:20])[CH:11]=[CH:10][C:4]=1[O:5][CH2:6][CH:7]1[O:9][CH2:8]1)#[N:2].[CH:22]([NH2:26])([CH2:24][CH3:25])[CH3:23]>C(O)C.C(OCC)(=O)C>[C:1]([C:3]1[CH:13]=[C:12]([NH:14][C:15](=[O:21])[CH2:16][CH2:17][CH2:18][CH2:19][CH3:20])[CH:11]=[CH:10][C:4]=1[O:5][CH2:6][CH:7]([OH:9])[CH2:8][NH:26][CH:22]([CH2:24][CH3:25])[CH3:23])#[N:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 24874Sec-ButylamineHCID 12939818HCID 12939818, 화합물

생성물 1

HCID 12764046HCID 12764046, 화합물수율 19%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 8857Ethyl Acetate용매

실험 절차

Ten grams (0.035 mol) of 1-(2-cyano-4-n-hexanoylamino-phenoxy)-2,3-epoxypropane were dissolved in 100 ml of ethanol, 7.3 gm (0.1 mol) of sec.butylamine were added, and the mixture was refluxed for one hour. After the solvent was distilled off in vacuo, the residue was purified by column chromatography in the manner described in Example 6. The base thus obtained was dissolved in ethyl acetate, washed with dilute NaOH and water, dried, and evaporated to dryness. The test substance remaining was recrystallized from ethyl acetate with the addition of petroleum ether. Subsequent recrystallization from acetonitrile yielded 2.4 gm of pure white crystalline base. M.p.: 72°-74° C.

후처리

  1. temperaturethe mixture was refluxed for one hour
  2. distillationAfter the solvent was distilled off in vacuo
  3. customthe residue was purified by column chromatography in the manner
  4. customThe base thus obtained
  5. washwashed with dilute NaOH and water
  6. customdried
  7. customevaporated to dryness
  8. customThe test substance remaining was recrystallized from ethyl acetate with the addition of petroleum ether
  9. customSubsequent recrystallization from acetonitrile

출처 및 근거

ORD 기록
ord-10c37181157040f6ae13a7971b958a10
출처 데이터셋
uspto-grants-1984_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04438143

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