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Water → HCID 20326670, 화합물

HRID 1288561
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HRID 1288561 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.C(=O)([O-])[O-].[K+].[K+].Cl[CH2:27][C:28]#[N:29].O>CN(C)C=O>[C:28]([CH2:27][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:29]
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참가 물질

6

반응물 4

HCID 962WaterHCID 7856ChloroacetonitrileHCID 11430Potassium CarbonateHCID 203266297,7-Diphenyl-1,4-oxazepane

생성물 1

HCID 20326670HCID 20326670, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

To the solution of 2.5 g of 7,7-diphenyl-hexahydro-1,4-oxazepine in 5 ml of dimethylformamide, 1.5 g of anhydrous potassium carbonate are added while stirring, followed by the dropwise addition of the solution of 0.85 g of chloroacetonitrile in 2 ml of dimethylformamide and the suspension is stirred for 5 hours at room temperature. It is poured onto a mixture of ice and water, the aqueous phase extracted twice with 20 ml of diethyl ether each, the extract dried, filtered and evaporated. The residue is recrystallized from ethanol, to yield the 4-cyanomethyl-7,7-diphenyl-hexahydro-1,4-oxazepine melting at 119°-121° (its hydrochloride melts at 178°-180° with decomposition).

후처리

  1. stirringthe suspension is stirred for 5 hours at room temperature
  2. extractionthe aqueous phase extracted twice with 20 ml of diethyl ether each, the extract
  3. customdried
  4. filtrationfiltered
  5. customevaporated
  6. customThe residue is recrystallized from ethanol

출처 및 근거

ORD 기록
ord-73b40cb4cfc34f9b9a9fbef44b31da12
출처 데이터셋
uspto-grants-1976_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03988448

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