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Sodium Iodide → HCID 22064705, 화합물

HRID 1828107
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HRID 1828107 반응식
[NH2:1][C:2]1[CH:10]=[C:9]2[C:5]([CH2:6][NH:7][C:8]2=[O:11])=[CH:4][CH:3]=1.[I-].[Na+].Br[CH2:15][CH2:16][CH2:17][CH2:18][CH2:19]Br.C(N(C(C)C)C(C)C)C>C(#N)C>[N:1]1([C:2]2[CH:10]=[C:9]3[C:5]([CH2:6][NH:7][C:8]3=[O:11])=[CH:4][CH:3]=2)[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]1
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6

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HCID 5238Sodium IodideHCID 81001,5-DibromopentaneHCID 81531DiisopropylethylamineHCID 220646276-Amino-2,3-dihydro-1H-isoindol-1-one

생성물 1

HCID 22064705HCID 22064705, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매

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온도
75 °C

실험 절차

6-Amino-2,3-dihydro-isoindol-1-one (0.810 g, CAS 675109-45-2) was dissolved in 12 ml of acetonitrile and treated successively with sodium iodide (2.458 g, 3 eq.), 1,5-dibromopentane (1.11 ml, 1.5 eq.), and N-ethyl-diisopropylamine (2.88 ml, 3.1 eq.), and the mixture was stirred at 75° C. for 20 h. Pouring onto crushed ice, twofold extraction with AcOEt, washing with water and brine, drying over magnesium sulfate, and evaporation of the solvents, followed by crystallization from hexane/ethyl acetate yielded 6-piperidin-1-yl-2,3-dihydro-isoindol-1-one (0.669 g) as light brown crystals, MS 217.3 ([M+H]+).

후처리

  1. additionPouring
  2. customonto crushed
  3. extractionice, twofold extraction with AcOEt
  4. washwashing with water and brine
  5. dry with materialdrying over magnesium sulfate, and evaporation of the solvents
  6. customfollowed by crystallization from hexane/ethyl acetate

출처 및 근거

ORD 기록
ord-e1993839da804100b5a2ad4238759003
출처 데이터셋
uspto-grants-2006_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07056932B2

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