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tert-Butyl piperazine-1-carboxylate → 1-(tert-Butoxycarbonyl)-4-[(6-methyl-4,5,6,7-tetrahydrothiazolo[5,4-c]pyridin-2-yl)carbonyl]piperazine

HRID 352873
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HRID 352873 반응식
[CH3:1][CH:2]1[NH:7][CH2:6][C:5]2[S:8][C:9]([C:11]([O-:13])=O)=[N:10][C:4]=2[CH2:3]1.[Li+].[C:15]([O:19][C:20]([N:22]1[CH2:27][CH2:26][NH:25][CH2:24][CH2:23]1)=[O:21])([CH3:18])([CH3:17])[CH3:16].O.ON1C2C=CC=CC=2N=N1.Cl.CN(C)CCCN=C=NCC>CN(C)C=O.O.C(Cl)Cl>[C:15]([O:19][C:20]([N:22]1[CH2:27][CH2:26][N:25]([C:11]([C:9]2[S:8][C:5]3[CH2:6][NH:7][CH:2]([CH3:1])[CH2:3][C:4]=3[N:10]=2)=[O:13])[CH2:24][CH2:23]1)=[O:21])([CH3:18])([CH3:16])[CH3:17]
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참가 물질

8

반응물 4

HCID 143452tert-Butyl piperazine-1-carboxylateHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 27960291-Hydroxybenzotriazole hydrateHCID 23674323Lithium 6-methyl-4,5,6,7-tetrahydrothiazolo[5,4-c]pyridine-2-carboxylate

생성물 1

HCID 227103621-(tert-Butoxycarbonyl)-4-[(6-methyl-4,5,6,7-tetrahydrothiazolo[5,4-c]pyridin-2-yl)carbonyl]piperazine

시약·촉매·용매 3

HCID 962Water용매HCID 6228Dimethylformamide용매HCID 6344Dichloromethane용매

실험 절차

To a solution of lithium 6-methyl-4,5,6,7-tetrahydrothiazolo[5,4-c]pyridine-2-carboxylate (293 mg) in N,N-dimethylformamide (10 ml) were added 1-(tert-butoxycarbonyl)piperazine (294 mg), 1-hydroxybenzotriazole monohydrate (214 mg) and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (303 mg) at room temperature. After stirring for 38 hours, methylene chloride (20 ml) and water (200 ml) were added to the reaction mixture to separate it into layers. The water layer thus obtained was extracted with methylene chloride (3×10 ml). The organic layers were combined, washed with a saturated aqueous solution (100 ml.) of sodium bicarbonate, dried over anhydrous sodium sulfate and distilled under reduced pressure to remove the solvent. The residue was purified by chromatography on a silica gel column (methylene chloride:acetone=2:1), whereby the title compound (300 mg) was obtained as a pale yellow viscous substance.

후처리

  1. customto separate it into layers
  2. customThe water layer thus obtained
  3. extractionwas extracted with methylene chloride (3×10 ml)
  4. washwashed with a saturated aqueous solution (100 ml.) of sodium bicarbonate
  5. dry with materialdried over anhydrous sodium sulfate
  6. distillationdistilled under reduced pressure
  7. customto remove the solvent
  8. customThe residue was purified by chromatography on a silica gel column (methylene chloride:acetone=2:1), whereby the title compound (300 mg)
  9. customwas obtained as a pale yellow viscous substance

출처 및 근거

ORD 기록
ord-972b48834fbd4c18bc7818c52705bf63
출처 데이터셋
uspto-grants-2004_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06747023B1

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