Triethylamine → HCID 14349013, 화합물

HRID 346058노트

반응식

HRID 346058 반응식
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]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 62324Propionyl chlorideHCID 14348987HCID 14348987, 화합물

생성물 1

HCID 14349013HCID 14349013, 화합물

시약·촉매·용매 1

HCID 6212Chloroform용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-3f180900e74a42f091cb878c66ce0e61
출처 데이터셋
uspto-grants-1991_10
특허 번호
US05059688

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