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Potassium Carbonate → HCID 70542436, 화합물

HRID 1112283
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HRID 1112283 반응식
Cl[CH2:2][CH:3]1[CH2:7][N:6]([CH:8]([CH3:10])[CH3:9])[C:5](=[O:11])[C:4]1([C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1.[OH:24][C:25]1([C:31]2[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=2)[CH2:30][CH2:29][NH:28][CH2:27][CH2:26]1.[C:37](=[O:40])([O-:39])[O-].[K+].[K+]>C(O)C>[C:5]([OH:24])(=[O:11])/[CH:4]=[CH:18]\[C:37]([OH:39])=[O:40].[C:18]1([C:4]2([C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=3)[CH:3]([CH2:2][N:28]3[CH2:27][CH2:26][C:25]([C:31]4[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=4)([OH:24])[CH2:30][CH2:29]3)[CH2:7][N:6]([CH:8]([CH3:10])[CH3:9])[C:5]2=[O:11])[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 963874-Phenylpiperidin-4-olHCID 12953546HCID 12953546, 화합물

생성물 1

HCID 70542436HCID 70542436, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of 15 g. (0.046 mole) of 4-chloromethyl-3,3-diphenyl-1-isopropyl-2-pyrrolidinone, 8.1 g. (0.046 mole) of 4-hydroxy-4-phenylpiperidine, 8.2 g. (0.06 mole) of potassium carbonate and 200 ml. of ethanol was heated in a steel bomb at 200° C. for 48 hours. The cooled mixture was partitioned between water and isopropyl ether. The dried isopropyl ether layer (sodium sulfate) was concentrated. The residual material (19 g.) was dissolved in 150 ml. of isopropyl alcohol to which solution was added 7.0 g of maleic acid and 50 ml. of isopropyl ether. The maleate salt was collected and recrystallized from isopropyl alcohol-water. The dried salt weighed 8.0 g and melted at 207°-208° C.

후처리

  1. additionA mixture of 15 g
  2. customThe cooled mixture was partitioned between water and isopropyl ether
  3. concentrationThe dried isopropyl ether layer (sodium sulfate) was concentrated
  4. dissolutionThe residual material (19 g.) was dissolved in 150 ml
  5. additionof isopropyl alcohol to which solution was added 7.0 g of maleic acid and 50 ml
  6. customThe maleate salt was collected
  7. customrecrystallized from isopropyl alcohol-water

출처 및 근거

ORD 기록
ord-6b1c41a2b2cc4c6c9e86bfabf79d2b49
출처 데이터셋
uspto-grants-1978_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04120969

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