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Sec-Butylamine → HCID 12764046、化合物

HRID 1903751
ノート
印刷プレビュー

反応式

HRID 1903751 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 24874Sec-ButylamineHCID 12939818HCID 12939818、化合物

生成物 1

HCID 12764046HCID 12764046、化合物収率 19%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-10c37181157040f6ae13a7971b958a10
出典データセット
uspto-grants-1984_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04438143

反応ノート

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