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Sodium Iodide → HCID 21418258, 화합물

HRID 441832
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HRID 441832 반응식
[C:1]1([C:7]2([C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=3)[O:13][CH2:12][CH2:11][NH:10][CH2:9][CH2:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.Cl[CH2:21][CH2:22][CH2:23][C:24]#[N:25].C(=O)([O-])[O-].[Na+].[Na+].[I-].[Na+]>CC(CC(=O)C)C>[C:24]([CH2:23][CH2:22][CH2:21][N:10]1[CH2:9][CH2:8][C:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)([C:14]2[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=2)[O:13][CH2:12][CH2:11]1)#[N:25]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 5238Sodium IodideHCID 10340Sodium CarbonateHCID 123364-ChlorobutyronitrileHCID 203266297,7-Diphenyl-1,4-oxazepane

생성물 1

HCID 21418258HCID 21418258, 화합물

시약·촉매·용매 1

HCID 7909Methyl Isobutyl Ketone용매

실험 절차

The mixture of 4.6 g of 7,7-diphenyl-hexahydro-1,4-oxazepine, 1.88 g of 4-chlorobutyronitrile, 1.88 g of anhydrous sodium carbonate, 0.3 g of sodium iodide and 60 ml of 2-methyl-4-pentanone is stirred at reflux for 23 hours and evaporated. The residue is partitioned between diethyl ether and water, the ethereal solution separated, washed with saturated aqueous sodium chloride, dried and evaporated, to give the 4-(3-cyanopropyl)-7,7-diphenyl-hexahydro-1,4-oxazepine melting at 89°-90°. (Analogously the 4-(4-cyanobutyl and 6-cyanohexyl)-7,7-diphenyl-hexahydro-1,4-oxazepines are prepared, melting at 67°-69° and showing an I.R. band at 2252cm-1 respectively).

후처리

  1. temperatureat reflux for 23 hours
  2. customevaporated
  3. customThe residue is partitioned between diethyl ether and water
  4. customthe ethereal solution separated
  5. washwashed with saturated aqueous sodium chloride
  6. customdried
  7. customevaporated

출처 및 근거

ORD 기록
ord-2bae4e14c42b4c3cbf84801d34ef504a
출처 데이터셋
uspto-grants-1977_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04042701

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