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Diisopropylamine → HCID 20314652, 화합물

HRID 2419857
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HRID 2419857 반응식
C(N[CH:5]([CH3:7])[CH3:6])(C)C.C([Li])CCC.[C:13]([O:18][CH3:19])(=[O:17])[CH:14]([CH3:16])[CH3:15].Br[CH2:21][C:22]1[CH:31]=[CH:30][C:29]2[C:24](=[CH:25][CH:26]=[C:27]([CH2:32]Br)[CH:28]=2)[CH:23]=1>O1CCCC1.CCCCCC>[C:13]([C:5]([CH3:6])([CH3:7])[CH2:21][C:22]1[CH:31]=[CH:30][C:29]2[C:24](=[CH:25][CH:26]=[C:27]([CH2:32][C:14]([CH3:16])([C:13]([O:18][CH3:19])=[O:17])[CH3:15])[CH:28]=2)[CH:23]=1)([O:18][CH3:19])=[O:17]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 7912DiisopropylamineHCID 11039Methyl isobutyrateHCID 36600102,6-Bis(bromomethyl)naphthaleneHCID 178418339Butyllithium

생성물 1

HCID 20314652HCID 20314652, 화합물

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매
HCID 8058
Hexane
용매

실험 절차

To a solution of 56 ml of diisopropylamine in 1200 ml of dry tetrahydrofuran at -78° C was added 260 ml of 1.6 M n-butyllithium in hexane. After 1 hr of stirring 40.4 g of methyl isobutyrate was added dropwise and the solution stirred for another 30 minutes. A 60-g portion of 2,6-bis(bromomethyl)naphthalene was added slowly, and the reaction mixture was stirred overnight and then brought to room temperature. Tetrahydrofuran was removed by evaporation. The residue was dissolved in 300 ml of chloroform, washed 3 times with 400 ml of H2O, dried and evaporated to dryness to obtain 56 g of 2,6-bis(2-carbomethoxy-2-methylpropyl)naphthalene, m.p. 108° C-110° C. The product was recrystallized from benzene.

후처리

  1. additionwas added dropwise
  2. stirringthe reaction mixture was stirred overnight
  3. custombrought to room temperature
  4. customTetrahydrofuran was removed by evaporation
  5. dissolutionThe residue was dissolved in 300 ml of chloroform
  6. washwashed 3 times with 400 ml of H2O
  7. customdried
  8. customevaporated to dryness

출처 및 근거

ORD 기록
ord-aaadaa96ddb348198062f05ee76a1ccf
출처 데이터셋
uspto-grants-1978_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04107444

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