Triethylamine → 4-(Benzoylamino)-N-[2-(N,N-dimethylamino)methyl-6-tetralinyl]benzamide

HRID 1242931노트

반응식

HRID 1242931 반응식
Cl.[NH2:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[CH2:9][CH:8]([CH2:13][N:14]([CH3:16])[CH3:15])[CH2:7][CH2:6]2.[C:17]([NH:25][C:26]1[CH:34]=[CH:33][C:29]([C:30](O)=[O:31])=[CH:28][CH:27]=1)(=[O:24])[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1.C1C=CC2N(O)N=NC=2C=1.C(N(CC)CC)C>CN(C1C=CN=CC=1)C.C(OCC)(=O)C.C1COCC1.O.CN(C=O)C>[C:17]([NH:25][C:26]1[CH:27]=[CH:28][C:29]([C:30]([NH:2][C:3]2[CH:4]=[C:5]3[C:10](=[CH:11][CH:12]=2)[CH2:9][CH:8]([CH2:13][N:14]([CH3:16])[CH3:15])[CH2:7][CH2:6]3)=[O:31])=[CH:33][CH:34]=1)(=[O:24])[C:18]1[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=1

참가 물질

9

반응물 4

HCID 8471TriethylamineHCID 757711-HydroxybenzotriazoleHCID 2525974-(Benzoylamino)benzoic acidHCID 219397736-Amino-2-(N,N-dimethylamino)methyltetralin hydrochloride

생성물 1

HCID 219397304-(Benzoylamino)-N-[2-(N,N-dimethylamino)methyl-6-tetralinyl]benzamide수율 84.4%

시약·촉매·용매 4

HCID 142844-(Dimethylamino)pyridine촉매HCID 962Water용매HCID 6228Dimethylformamide용매HCID 21939870Tetrahydrofuran ethyl acetate용매

실험 절차

6-Amino-2-(N,N-dimethylamino)methyltetralin hydrochloride (139 mg), 4-benzoylaminobenzoic acid (121 mg), WSCD (0.13 ml), HOBt (92 mg), triethylamine (0.14 ml) and DMAP (61 mg) were added to DMF (4 ml). After the reaction mixture was shaken at room temperature for 20 hours using a shaker, the reaction mixture was poured into water, and extraction was conducted using ethyl acetate-THF (1:1). The organic layer was washed with water, saturated sodium bicarbonate solution and saturated aqueous sodium chloride solution, dried, and then concentrated. The resulting crude crystal was washed with hexane, to give the titled compound (181 mg).

후처리

  1. washThe organic layer was washed with water, saturated sodium bicarbonate solution and saturated aqueous sodium chloride solution
  2. customdried
  3. concentrationconcentrated
  4. washThe resulting crude crystal was washed with hexane

출처 및 근거

ORD 기록
ord-86da2f95597a466a86901b039b379cdf
출처 데이터셋
uspto-grants-2006_10
특허 번호
US07115750B1

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