Morpholine → HCID 178420829、化合物

HRID 36732

反応式

HRID 36732 の反応式
[C:1]([C:5]1[CH:6]=[C:7]([CH:18]=[C:19]([C:22]([CH3:25])([CH3:24])[CH3:23])[C:20]=1[OH:21])[NH:8][C:9]1[CH:10]=[C:11]([CH:15]=[CH:16][CH:17]=1)[C:12]([OH:14])=[O:13])([CH3:4])([CH3:3])[CH3:2].[NH:26]1[CH2:31][CH2:30][O:29][CH2:28][CH2:27]1>C(O)(C)C>[NH2+:26]1[CH2:31][CH2:30][O:29][CH2:28][CH2:27]1.[C:22]([C:19]1[CH:18]=[C:7]([CH:6]=[C:5]([C:1]([CH3:4])([CH3:3])[CH3:2])[C:20]=1[OH:21])[NH:8][C:9]1[CH:10]=[C:11]([CH:15]=[CH:16][CH:17]=1)[C:12]([O-:14])=[O:13])([CH3:25])([CH3:24])[CH3:23]

参加物

4

反応物 2

HCID 8083MorpholineHCID 601943-(3,5-DI-T-Butyl-4-hydroxyanilino)benzoic acid

生成物 1

HCID 178420829HCID 178420829、化合物

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒2 回

実験手順

A mixture of 1.70 g (0.005 mole) of 3-(3,5-di-tertiary-butyl-4-hydroxyanilino)benzoic acid (prepared in Example 13) and 50 ml of hot isopropyl alcohol was filtered to remove a small amount of insoluble material. The resulting solution was deoxygenated with a stream of nitrogen gas. Uner a nitrogen atmosphere, a solution of 0.44 g (0.005 mole) of morpholine in 1.5 ml of isopropyl alcohol was added with rapid stirring. Evaporation provided a solid which was recrystallized from a mixture of isopropyl alcohol and isopropyl ether to give solid morpholinium-3-(3,5-di-tertiary-butyl-4-hydroxyanilino)benzoate, m.p. 147°-150° C. Analysis: Calculated for C21H27NO3C4H9NO: % C, 70.1; % H, 8.5; % N, 6.5; Found: % C, 69.8; % H, 8.5; % N, 6.4.

後処理

  1. filtrationwas filtered
  2. customto remove a small amount of insoluble material
  3. customThe resulting solution was deoxygenated with a stream of nitrogen gas
  4. customEvaporation
  5. customprovided a solid which
  6. customwas recrystallized from a mixture of isopropyl alcohol and isopropyl ether

出典と根拠

ORDレコード
ord-e1edbfdaf3444622a6b2528ed1990c0f
出典データセット
uspto-grants-1995_05
特許番号
US05416113

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