Triethylamine → HCID 14349021, 화합물

HRID 346061노트

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HRID 346061 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 14349021HCID 14349021, 화합물

시약·촉매·용매 1

HCID 6212Chloroform용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-c72b842621d14b1aac90c2064d0b9a55
출처 데이터셋
uspto-grants-1991_10
특허 번호
US05059688

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