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Dichloromethane → N-(Tetrahydro-2H-pyran-2-yloxy) 2-{6-[(naphthalene-2-sulfonyl)-(2-pyrrolidin-1-ylethyl)amino]-3-azabicyclo[3.1.0]hex-3-yl}pyrimidine-5-carboxamide

HRID 2079786
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HRID 2079786 반응식
[H-].[Na+].[O:3]1[CH2:8][CH2:7][CH2:6][CH2:5][CH:4]1[O:9][NH:10][C:11]([C:13]1[CH:14]=[N:15][C:16]([N:19]2[CH2:24][CH:23]3[CH:21]([CH:22]3[NH:25][S:26]([C:29]3[CH:38]=[CH:37][C:36]4[C:31](=[CH:32][CH:33]=[CH:34][CH:35]=4)[CH:30]=3)(=[O:28])=[O:27])[CH2:20]2)=[N:17][CH:18]=1)=[O:12].Cl.Cl[CH2:41][CH2:42][N:43]1[CH2:47][CH2:46][CH2:45][CH2:44]1.C(Cl)Cl>CCCCCCC.CN(C=O)C>[O:3]1[CH2:8][CH2:7][CH2:6][CH2:5][CH:4]1[O:9][NH:10][C:11]([C:13]1[CH:14]=[N:15][C:16]([N:19]2[CH2:20][CH:21]3[CH:23]([CH:22]3[N:25]([S:26]([C:29]3[CH:38]=[CH:37][C:36]4[C:31](=[CH:32][CH:33]=[CH:34][CH:35]=4)[CH:30]=3)(=[O:27])=[O:28])[CH2:41][CH2:42][N:43]3[CH2:47][CH2:46][CH2:45][CH2:44]3)[CH2:24]2)=[N:17][CH:18]=1)=[O:12]
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반응물 4

HCID 6344DichloromethaneHCID 24758Sodium hydride2회HCID 816681-(2-Chloroethyl)pyrrolidine hydrochlorideHCID 59367684N-(Tetrahydro-2H-pyran-2-yloxy) 2-[6-(naphthalene-2-sulfonylamino)-3-azabicyclo[3.1.0]hex-3-yl]pyrimidine-5-carboxamide2회

생성물 1

HCID 59367676
N-(Tetrahydro-2H-pyran-2-yloxy) 2-{6-[(naphthalene-2-sulfonyl)-(2-pyrrolidin-1-ylethyl)amino]-3-azabicyclo[3.1.0]hex-3-yl}pyrimidine-5-carboxamide
수율 19.8%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매2회HCID 8900Heptane용매

실험 절차

NaH (0.223 g, 5.5 mmol) was washed with heptane (10 ml), then suspended in DMF (5 ml). N-(Tetrahydro-2H-pyran-2-yloxy) 2-{6-[(naphthalene-2-sulfonyl)amino]-3-azabicyclo[3.1.0]hex-3-yl}pyrimidine-5-carboxamide (0.991 g, 1.95 mmol) was added, and the mixture stirred for 5 min. To NaH (0.172 g, 4.3 mmol) in DMF was added 1-(2-chloroethyl)-pyrrolidine hydrochloride (0.724 g, 4.2 mmol). The reaction was swirled gently for 2 min, and then added to the solution of N-(tetrahydro-2H-pyran-2-yloxy) 2-{6-[(naphthalene-2-sulfonyl)amino]-3-azabicyclo[3.1.0]hex-3-yl}pyrimidine-5-carboxamide. The mixture was stirred at r.t. for 5 days, then poured into DCM (150 ml) and quenched with 2.4M ammonium chloride solution (50 ml). The organic layer was separated, and the aqueous was further extracted with DCM (150 ml). The combined organic extracts were dried, concentrated in vacuo to give the title compound (0.234 g, 19%). This was carried forward without further purification.

후처리

  1. waitThe reaction was swirled gently for 2 min
  2. stirringThe mixture was stirred at r.t. for 5 days
  3. customquenched with 2.4M ammonium chloride solution (50 ml)
  4. customThe organic layer was separated
  5. extractionthe aqueous was further extracted with DCM (150 ml)
  6. customThe combined organic extracts were dried
  7. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-75ec557e165645dd98d93dc90fcc1e5b
출처 데이터셋
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07932246B2

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