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Hydrochloric Acid → HCID 13389105, 화합물

HRID 746282
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HRID 746282 반응식
[C:1]1([CH:7]2[CH2:11][N:10]3[CH2:12][CH2:13][CH2:14][C:9]3=[N:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[Li]CCCC.[Cl:20]C1C=CC=C(Cl)C=1S[S:29][C:30]1[C:35]([Cl:36])=[CH:34][CH:33]=[CH:32][C:31]=1[Cl:37].Cl>>[ClH:20].[C:1]1([CH:7]2[CH2:11][N:10]3[CH2:12][CH2:13][CH:14]([S:29][C:30]4[C:31]([Cl:37])=[CH:32][CH:33]=[CH:34][C:35]=4[Cl:36])[C:9]3=[N:8]2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 4

HCID 313Hydrochloric AcidHCID 588476Disulfide, bis(2,6-dichlorophenyl)-HCID 12258399HCID 12258399, 화합물HCID 178418339Butyllithium

생성물 1

HCID 13389105HCID 13389105, 화합물수율 40.7%

실험 절차

2,5,6,7-Tetrahydro-2-phenyl-3H-pyrrolo[1,2-a]imidazole was reacted with 2 equivalents of n-BuLi and 1 equivalent of 2,6-dichlorophenyldisulfide according to the general procedure A above except that when the reaction mixture was poured into the aq HCl solution, the HCl salt of the desired product precipitated. It was collected, washed well with cold H2O, then Et2O and dried in vacuo; yield 40.7%; m.p. 96°-99°. Neutralization of the acidic filtrate with NaHCO3, followed by extraction with Et2O, yielded an additional amount of the desired product as the free base (39.2%).

후처리

  1. customthe HCl salt of the desired product precipitated
  2. customIt was collected
  3. washwashed well with cold H2O
  4. dry with materialEt2O and dried in vacuo
  5. extractionNeutralization of the acidic filtrate with NaHCO3, followed by extraction with Et2O

출처 및 근거

ORD 기록
ord-22ca92444df94fae87d7525e13d5e09b
출처 데이터셋
uspto-grants-1986_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04603206

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