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tert-Butyl piperazine-1-carboxylate → HCID 69420014, 화합물

HRID 1373635
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HRID 1373635 반응식
Br[C:2]1[CH:11]=[CH:10][CH:9]=[C:8]2[C:3]=1[CH2:4][CH2:5][O:6][CH2:7]2.[C:12]([N:19]1[CH2:24][CH2:23][NH:22][CH2:21][CH2:20]1)([O:14][C:15]([CH3:18])([CH3:17])[CH3:16])=[O:13].CC([O-])(C)C.[Na+]>CC([O-])=O.CC([O-])=O.[Pd+2].C1(P(C2CCCCC2)C2C=CC=CC=2C2C=CC=CC=2)CCCCC1>[C:15]([O:14][C:12]([N:19]1[CH2:24][CH2:23][N:22]([C:2]2[CH:11]=[CH:10][CH:9]=[C:8]3[C:3]=2[CH2:4][CH2:5][O:6][CH2:7]3)[CH2:21][CH2:20]1)=[O:13])([CH3:18])([CH3:16])[CH3:17]
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참가 물질

6

반응물 3

HCID 143452tert-Butyl piperazine-1-carboxylateHCID 107986265-bromo-3,4-dihydro-1H-2-benzopyranHCID 23676156Sodium t-butoxide

생성물 1

HCID 69420014HCID 69420014, 화합물수율 60%

시약·촉매·용매 2

HCID 167845palladium(II) acetate촉매
HCID 2734216
2-(Dicyclohexylphosphino)biphenyl
촉매

실험 절차

A third intermediate compound, 1-Isochroman-5-yl-piperazine, was produced as follows: To a mixture of 5-bromo-isochroman (1 g, 4.69 mmol), 1-boc-piperazine (1.05 g, 5.6 mmol), 2-dicyclohexylphosphino biphenyl (0.066 g, 0.19 mmol), and Pd(OAc)2 (0.42 g, 0.19 mmol) in 10 mL of dry degassed C6H5CH3 was added NaOtBu (0.63 g, 6.6 mmol) at room temperature. The resulting mixture was stirred at 80–90° C. for 1 h, cooled and passed through a pad of celite and the filtrate was concentrated under vacuum. The residue was purified by chromatography (25–50% EtOAc/hexanes) to give 4-isochroman-5-yl-piperazine-1-carboxylic acid tert-butyl ester (0.89 g, 60%). MS (ES) m/z: 319.19 [M+1]. 1H NMR (400 MHz, CDCl3) δ 7.16 (t, J=7.8 Hz, 1H), 6.88 (d, J=7.8 Hz, 1H), 6.75 (d, J=7.8 Hz, 1H), 4.79 (s, 2H), 3.94 (t, J=5.9 Hz, 2H), 3.55 (br s, 4H), 2.86–2.80 (m, 4H), 1.49 (s, 9H).

후처리

  1. customof dry
  2. customdegassed C6H5CH3
  3. temperaturecooled
  4. concentrationthe filtrate was concentrated under vacuum
  5. customThe residue was purified by chromatography (25–50% EtOAc/hexanes)

출처 및 근거

ORD 기록
ord-6e0f2b885c484435b913704431c99200
출처 데이터셋
uspto-grants-2007_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07160888B2

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