Acetic Acid → HCID 178418702, 화합물

HRID 1884442

반응식

HRID 1884442 반응식
[N+:1]([C:4]1[CH:16]=[CH:15][C:7]([CH2:8][N:9]2[CH2:14][CH2:13][CH2:12][CH2:11][CH2:10]2)=[CH:6][CH:5]=1)([O-])=O.Cl.[OH-:18].[Na+].N1([CH2:26][NH:27][C:28]2[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=2)CCCCC1.[C:34](O)(=O)[CH3:35]>O>[N:9]1([CH2:8][C:7]2[CH:15]=[CH:16][C:4]([NH:1][CH:34]=[C:35]3[C:29]4[C:28](=[CH:33][CH:32]=[CH:31][CH:30]=4)[NH:27][C:26]3=[O:18])=[CH:5][CH:6]=2)[CH2:14][CH2:13][CH2:12][CH2:11][CH2:10]1

참가 물질

7

반응물 5

HCID 176Acetic AcidHCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 7835411-(4-Nitrobenzyl)piperidineHCID 21974891Piperidin-1-ylmethyl-phenylamine

생성물 1

HCID 178418702HCID 178418702, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

1-(4-Nitro-benzyl)-piperidine (0.5052 gms.) is suspended in 25 mL of a 1:1 (v:v) solution of acetic acid and water. The suspension is then treated with 45 mL of an ˜10 wt. % solution of TiCl3 in 20-30 wt. % HCl, dropwise. Over the course of the addition a color change from colorless to purple to black ensues. The reaction mixture is immersed in a 60° C. oil bath overnight following the addition of TiCl3. The reaction mixture is then cooled to room temperature and made basic with the addition of a 10% aqueous solution of NaOH. The basic reaction mixture is extracted with chloroform, and the organic layer is dried over anhydrous sodium sulfate. Following evaporation of the solvent the organic layer yields 0.333 gms. of piperidin-1-ylmethyl-phenylamine.

후처리

  1. additionOver the course of the addition a color change from colorless to purple to black ensues
  2. customis immersed in a 60° C.
  3. customovernight
  4. customThe basic reaction mixture
  5. extractionis extracted with chloroform
  6. dry with materialthe organic layer is dried over anhydrous sodium sulfate
  7. customevaporation of the solvent the organic layer
  8. customyields 0.333 gms

출처 및 근거

ORD 기록
ord-625151de875c4f5d96fe2ab485dfd3eb
출처 데이터셋
uspto-grants-2004_07
특허 번호
US06765012B2

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