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Acetate → HCID 66581119, 화합물

HRID 1521853
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HRID 1521853 반응식
I[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C([O-])(=O)C.[CH:12]1[N:20]2[C:15]([CH2:16][S:17][C:18]3[CH:24]=[CH:23][CH:22]=[CH:21][C:19]=32)=[C:14]([C:25]([O:27][CH2:28][CH3:29])=[O:26])[N:13]=1>CN(C=O)C.C(Cl)Cl.[Pd]>[C:2]1([C:12]2[N:20]3[C:15]([CH2:16][S:17][C:18]4[CH:24]=[CH:23][CH:22]=[CH:21][C:19]=43)=[C:14]([C:25]([O:27][CH2:28][CH3:29])=[O:26])[N:13]=2)[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 3

HCID 175AcetateHCID 11575IodobenzeneHCID 19836752HCID 19836752, 화합물

생성물 1

HCID 66581119HCID 66581119, 화합물수율 31%

시약·촉매·용매 3

HCID 23938Palladium촉매HCID 6228Dimethylformamide용매
HCID 6344
Dichloromethane
용매

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온도
140 °C

실험 절차

Iodo benzene (0.15 mL, 1.15 mmol, 2 eq), palladium (Il) acetate (6.4 mg, 0.03 mmol, 0.05 eq), and Cul (0.22 g, 1.15 mmol, 2 eq) are taken in pressure tube to which is added ethyl 4H-imidazo[5,1-c][1,4]benzothiazine-3-carboxylate (0.15 g, 0.576 mmol, 1 eq) taken in degassed DMF (6 mL) and the contents are heated at 140° C. for 12 h. The reaction mixture is diluted with DCM and filtered through celite. The filtrate is concentrated, passed through a plug of silica gel and concentrated to get the crude product 60 mg which is taken as such to next step. MS (ESI+): 337.2.

후처리

  1. filtrationfiltered through celite
  2. concentrationThe filtrate is concentrated
  3. concentrationconcentrated

출처 및 근거

ORD 기록
ord-863e1e3f58c9463fb54bef66eb778ea5
출처 데이터셋
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09073940B2

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