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Triethylamine → HCID 58447051, 화합물

HRID 1045778
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HRID 1045778 반응식
[Br:1][C:2]1[C:3]2[N:4]([N:9]=[N:10][N:11]=2)[C:5](Cl)=[N:6][CH:7]=1.[N:12]1([C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19])[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]1.C(N(CC)CC)C>C(O)C>[Br:1][C:2]1[C:3]2[N:4]([N:9]=[N:10][N:11]=2)[C:5]([N:15]2[CH2:14][CH2:13][N:12]([C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19])[CH2:17][CH2:16]2)=[N:6][CH:7]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 143452tert-Butyl piperazine-1-carboxylateHCID 58447058HCID 58447058, 화합물

생성물 1

HCID 58447051HCID 58447051, 화합물수율 94%

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
30 °C

실험 절차

A 250 mL round bottom flask was charged with 8-bromo-5-chlorotetrazolo[1,5-c]pyrimidine (10 g, 42.7 mmol), tert-butyl piperazine-1-carboxylate (11.9 g, 64 mmol), triethylamine (13 g, 0.13 mol) and ethanol (200 mL). The resulting mixture was heated at 30° C. for 2 h under N2 and then cooled to room temperature. The mixture was concentrated under reduced pressure to dryness. The residue was diluted with water (20 mL) and extracted with dichloromethane (20 mL×3). The combined organic layers were washed with brine (20 mL), dried over anhydrous Na2SO4 and concentrated in vacuo, to afford 15.4 g (94%) of the product as an off-white solid.

후처리

  1. temperaturecooled to room temperature
  2. concentrationThe mixture was concentrated under reduced pressure to dryness
  3. additionThe residue was diluted with water (20 mL)
  4. extractionextracted with dichloromethane (20 mL×3)
  5. washThe combined organic layers were washed with brine (20 mL)
  6. dry with materialdried over anhydrous Na2SO4
  7. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-675c22fa3f1447298249b221403d11a7
출처 데이터셋
uspto-grants-2013_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08569300B2

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