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Potassium tert-butoxide → HCID 68155891, 화합물

HRID 1877792
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HRID 1877792 반응식
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([Cl:8])=[CH:4][C:3]=1[CH2:9][N:10]1[CH:14]=[C:13]([CH3:15])[CH:12]=[C:11]1[C:16]([O:18]CC)=O.CC(C)([O-])C.[K+]>CS(C)=O>[Cl:8][C:5]1[CH:6]=[CH:7][C:2]2[NH:1][C:16](=[O:18])[C:11]3=[CH:12][C:13]([CH3:15])=[CH:14][N:10]3[CH2:9][C:3]=2[CH:4]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 23665647Potassium tert-butoxideHCID 68155862ethyl 1-(2-amino-5-chlorobenzyl)-4-methyl-1H-pyrrole-2-carboxylate

생성물 1

HCID 68155891HCID 68155891, 화합물수율 91%

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

반응 조건

온도
80 °C

실험 절차

To a solution of ethyl 1-[(2-amino-5-chloro-phenyl)methyl]-4-methyl-pyrrole-2-carboxylate (35 g, 119.55 mmoles) in dimethyl sulfoxide (120 mL) add potassium t-butoxide (14.76 g, 131.5 mmoles) over 10 minutes. Heat at 80° C. (oil-bath temperature) for 1 h. Allow to cool then pour onto water (400 mL). Collect the resulting brown powdery solid by filtration, washing well with water. Suck as dry as possible on the sinter then transfer to a dish and dry in a vacuum oven at 55° C. over phosphorus pentoxide overnight, to give 7-chloro-2-methyl-5,10-dihydro-11H-pyrrolo[2,1-c][1,4]benzodiazepin-11-one (22 g, 91%). MS (m/z): 247.1 (M+1).

후처리

  1. temperatureto cool
  2. additionthen pour onto water (400 mL)
  3. customCollect the resulting brown powdery solid
  4. filtrationby filtration
  5. washwashing well with water
  6. customSuck as dry as possible on the sinter
  7. dry with materialdry in a vacuum oven at 55° C. over phosphorus pentoxide overnight

출처 및 근거

ORD 기록
ord-b35f43b6d9814d328bf7942d0d9dd0ad
출처 데이터셋
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08314092B2

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