Triethylamine → HCID 14349021、化合物

HRID 346061ノート

反応式

HRID 346061 の反応式
[F:1][C:2]([F:22])([F:21])[C:3]1[CH:20]=[CH:19][C:6]([O:7][CH:8]2[C:14]3[CH:15]=[CH:16][CH:17]=[CH:18][C:13]=3[CH2:12][CH2:11][NH:10][CH2:9]2)=[CH:5][CH:4]=1.[CH2:23]([N:25](CC)CC)[CH3:24].Cl[C:31]([O:33][CH2:34][CH3:35])=[O:32]>C(Cl)(Cl)Cl>[CH2:34]([O:33][C:31]([NH:25][CH2:23][CH2:24][N:10]1[CH2:9][CH:8]([O:7][C:6]2[CH:19]=[CH:20][C:3]([C:2]([F:1])([F:21])[F:22])=[CH:4][CH:5]=2)[C:14]2[CH:15]=[CH:16][CH:17]=[CH:18][C:13]=2[CH2:12][CH2:11]1)=[O:32])[CH3:35]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 10928Ethyl chloroformateHCID 143489861-[4-(Trifluoromethyl)phenoxy]-2,3,4,5-tetrahydro-1H-3-benzazepine

生成物 1

HCID 14349021HCID 14349021、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 3-aminoethyl)-2,3,4,5-tetrahydro-1-(p-trifluoromethylphenoxy)-3-benzazepine of Example 21b (5.5 g, 0.016 mole) and triethylamine (1.8 g, 0.018 mole) in chloroform (75 ml) was slowly dropped a solution of ethyl chloroformate (2.0 g, 0.018 mole) in chloroform (25 ml). After stirring twenty hours at ambient temperature the reaction mixture was concentrated to a semisolid which was dissolved in ether, washed with water and dried (saturated NaCl, anhydrous MgSO4). The solution was filtered and concentrated to yield an oil. A sample of the resultant oil was distilled to yield an oil of 3-(2-ethoxycarbonylaminoethyl)-2,3,4,5-tetrahydro-1-(p-trifluoromethylphenoxy)-3-benzazepine, bp 235°-238° C./0.10 mm.

後処理

  1. concentrationwas concentrated to a semisolid which
  2. dissolutionwas dissolved in ether
  3. washwashed with water
  4. dry with materialdried (saturated NaCl, anhydrous MgSO4)
  5. filtrationThe solution was filtered
  6. concentrationconcentrated
  7. customto yield an oil
  8. distillationA sample of the resultant oil was distilled

出典と根拠

ORDレコード
ord-c72b842621d14b1aac90c2064d0b9a55
出典データセット
uspto-grants-1991_10
特許番号
US05059688

反応ノート

読み込み中…