4-(Trifluoromethyl)benzoyl chloride → 6-chloro-7,8-dihydroxy-1-phenyl-3-(p-trifluoromethylbenzoyl)-2,3,4,5-tetrahydro-1H-3-benzazepine

HRID 2198753

반응식

HRID 2198753 반응식
Cl.[Cl:2][C:3]1[C:13]2[CH2:12][CH2:11][NH:10][CH2:9][CH:8]([C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=3)[C:7]=2[CH:6]=[C:5]([OH:20])[C:4]=1[OH:21].[F:22][C:23]([F:34])([F:33])[C:24]1[CH:32]=[CH:31][C:27]([C:28](Cl)=[O:29])=[CH:26][CH:25]=1.C(=O)(O)[O-].[Na+]>CC(C)=O.O>[Cl:2][C:3]1[C:13]2[CH2:12][CH2:11][N:10]([C:28](=[O:29])[C:27]3[CH:31]=[CH:32][C:24]([C:23]([F:22])([F:33])[F:34])=[CH:25][CH:26]=3)[CH2:9][CH:8]([C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=3)[C:7]=2[CH:6]=[C:5]([OH:20])[C:4]=1[OH:21]

참가 물질

5

반응물 3

HCID 676074-(Trifluoromethyl)benzoyl chlorideHCID 516892Sodium BicarbonateHCID 9927337HCID 9927337, 화합물

생성물 1

HCID 129097606-chloro-7,8-dihydroxy-1-phenyl-3-(p-trifluoromethylbenzoyl)-2,3,4,5-tetrahydro-1H-3-benzazepine

시약·촉매·용매 1

HCID 18366337Propan-2-one--water (1/1)용매

실험 절차

A solution of 0.74 g (0.002 mole) of 6-chloro-7,8-dihydroxy-1-phenyl-2,3,4,5-tetrahydro-1H-3-benzazepine hydrochloride, 0.55 g (0.0025 mole) of p-trifluoromethyl benzoylchloride, 0.17 g (0.002 mole) of sodium bicarbonate and 40 ml of 1:1 acetone-water solution was stirred overnight under nitrogen. The mixture was evaporated to dryness. The residue was extracted with ethylacetate. The extracted material was purified over a silica gel column using methanol-ethyl acetate to give 6-chloro-7,8-dihydroxy-1-phenyl-3-(p-trifluoromethylbenzoyl)-2,3,4,5-tetrahydro-1H-3-benzazepine, m.p. 243°-245° (dec.).

후처리

  1. customThe mixture was evaporated to dryness
  2. extractionThe residue was extracted with ethylacetate
  3. customThe extracted material was purified over a silica gel column

출처 및 근거

ORD 기록
ord-cac9678630b446bb91795ad1791a8463
출처 데이터셋
uspto-grants-1982_11
특허 번호
US04359464

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