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Potassium Carbonate → HCID 86735776, 화합물

HRID 839714
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HRID 839714 반응식
[N:1]1([CH2:7][CH2:8][O:9][CH:10]2[CH2:14][CH2:13][NH:12][CH2:11]2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.Cl[CH2:16][CH2:17][N:18]1[CH2:23][CH2:22][CH2:21][CH2:20][CH2:19]1.C(=O)([O-])[O-].[K+].[K+].O.O.[C:32]([OH:37])(=[O:36])[C:33]([OH:35])=[O:34]>C1C=CC=CC=1>[C:32]([OH:37])(=[O:36])[C:33]([OH:35])=[O:34].[C:32]([OH:37])(=[O:36])[C:33]([OH:35])=[O:34].[C:32]([OH:37])(=[O:36])[C:33]([OH:35])=[O:34].[N:18]1([CH2:17][CH2:16][N:12]2[CH2:13][CH2:14][CH:10]([O:9][CH2:8][CH2:7][N:1]3[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]3)[CH2:11]2)[CH2:23][CH2:22][CH2:21][CH2:20][CH2:19]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 11430Potassium CarbonateHCID 61373Oxalic acid dihydrateHCID 748271-(2-Chloroethyl)piperidineHCID 2133316470001-70-6

생성물 1

HCID 86735776HCID 86735776, 화합물수율 32%

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

A solution of 10.0 g. (0.051 mole) of 3-(2-piperidinoethoxy)pyrrolidine and 10.4 g. (0.07 mole) of 1-(2-chloroethyl)piperidine in 200 ml. dry benzene was stirred with 28 g. (0.2 mole) of potassium carbonate at reflux for 15 hr. After cooling, the reaction mixture was filtered and concentrated. The residual oil was molecularly distilled to give a slightly impure product which when treated with three equivalents of oxalic acid dihydrate gave 9.3 g. of the trioxalate salt, m.p. 155°-162° C. (32% yield). The salt was recrystallized from methanol to give 5.8 g. of white crystalline salt, m.p. 177°-179° C.

후처리

  1. temperatureAfter cooling
  2. filtrationthe reaction mixture was filtered
  3. concentrationconcentrated
  4. distillationThe residual oil was molecularly distilled
  5. customto give a slightly impure product which when
  6. customgave 9.3 g
  7. customThe salt was recrystallized from methanol
  8. customto give 5.8 g

출처 및 근거

ORD 기록
ord-9b37900ae68a429da2e68e89059afa45
출처 데이터셋
uspto-grants-1978_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04096331

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