Triethylamine → HCID 14349013、化合物

HRID 346058ノート

反応式

HRID 346058 の反応式
C(O)(=O)C(O)=O.[F:7][C:8]([F:28])([F:27])[C:9]1[CH:26]=[CH:25][C:12]([O:13][CH:14]2[C:20]3[CH:21]=[CH:22][CH:23]=[CH:24][C:19]=3[CH2:18][CH2:17][NH:16][CH2:15]2)=[CH:11][CH:10]=1.C(N(CC)CC)C.[C:36](Cl)(=[O:39])[CH2:37][CH3:38]>C(Cl)(Cl)Cl>[C:36]([N:16]1[CH2:15][CH:14]([O:13][C:12]2[CH:25]=[CH:26][C:9]([C:8]([F:7])([F:27])[F:28])=[CH:10][CH:11]=2)[C:20]2[CH:21]=[CH:22][CH:23]=[CH:24][C:19]=2[CH2:18][CH2:17]1)(=[O:39])[CH2:37][CH3:38]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 62324Propionyl chlorideHCID 14348987HCID 14348987、化合物

生成物 1

HCID 14349013HCID 14349013、化合物

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒2 回

実験手順

To a cooled solution of 2,3,4,5-tetrahydro-1-(p-trifluoromethylphenoxy)-3-benzazpine of Example 1 (6.5 g, 0.021 mole) and triethylamine (2.5 g, 0.025 mole) in chloroform (75 ml) was slowly dropped propionyl chloride (2.3 g, 0.025 mole) in chloroform (10 ml). After stirring at ambient temperature two hours the reaction mixture was concentrated to an oil which was dissolved in ether then washed with water, dilute HCl, again twice with water and dried (saturated NaCl, anhydrous MgSO4). The solution was filtered then concentrated to a solid (7.2 g, 95%, m.p. 98°-105° C.). A sample was twice recrystallized from hexanes to yield 3-propionyl-2,3,4,5-tetrahydro-1-(p-trifluoromethylphenoxy)-3-benzazepine, m.p. 109°-110° C.

後処理

  1. concentrationwas concentrated to an oil which
  2. dissolutionwas dissolved in ether
  3. washthen washed with water, dilute HCl, again twice with water
  4. dry with materialdried (saturated NaCl, anhydrous MgSO4)
  5. filtrationThe solution was filtered
  6. concentrationthen concentrated to a solid (7.2 g, 95%, m.p. 98°-105° C.)
  7. customA sample was twice recrystallized from hexanes

出典と根拠

ORDレコード
ord-3f180900e74a42f091cb878c66ce0e61
出典データセット
uspto-grants-1991_10
特許番号
US05059688

反応ノート

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