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Dichloromethane → HCID 68614655, 화합물

HRID 1943244
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HRID 1943244 반응식
[NH2:1][CH2:2][C@@H:3]1[CH2:7][CH2:6][N:5]([CH2:8][C@H:9]2[N:19]3[C:20]4[N:11]([C:12](=[O:22])[CH:13]=[CH:14][C:15]=4[CH:16]=[CH:17][C:18]3=[O:21])[CH2:10]2)[CH2:4]1.[S:23]1[C:31]2[CH:30]=[C:29]([CH:32]=O)[N:28]=[CH:27][C:26]=2[O:25][CH2:24]1.S([O-])([O-])(=O)=O.[Na+].[Na+].C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].C(Cl)[Cl:56]>CO.CO.C(Cl)Cl>[ClH:56].[ClH:56].[S:23]1[C:31]2[CH:30]=[C:29]([CH2:32][NH:1][CH2:2][C@@H:3]3[CH2:7][CH2:6][N:5]([CH2:8][C@H:9]4[N:19]5[C:20]6[N:11]([C:12](=[O:22])[CH:13]=[CH:14][C:15]=6[CH:16]=[CH:17][C:18]5=[O:21])[CH2:10]4)[CH2:4]3)[N:28]=[CH:27][C:26]=2[O:25][CH2:24]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 5

HCID 6344DichloromethaneHCID 24436Sodium SulfateHCID 5049666Sodium triacetoxyborohydrideHCID 59254367[1,3]Oxathiolo[5,4-c]pyridine-6-carbaldehydeHCID 68596242HCID 68596242, 화합물

생성물 1

HCID 68614655HCID 68614655, 화합물

시약·촉매·용매 2

HCID 887Methanol용매
HCID 21226129Dichloromethane methanol용매

실험 절차

To a 10 mL round-bottomed flask were added (1R)-1-{[(3S)-3-(aminomethyl)-1-pyrrolidinyl]methyl}-1,2-dihydro-4H,9H-imidazo[1,2,3-ij]-1,8-naphthyridine-4,9-dione (60 mg, 0.200 mmol), [1,3]oxathiolo[5,4-c]pyridine-6-carbaldehyde (33.4 mg, 0.200 mmol) (for a synthesis see WO2004058144 Example 61), and sodium sulfate (250 mg, 1.760 mmol) in DCM (4 ml) and methanol (1.00 ml) to give an orange suspension. The reaction was stirred overnight under nitrogen. Sodium triacetoxyborohydride (85 mg, 0.400 mmol) was added and the reaction was stirred for 3 h. The reaction mixture was diluted with 10% MeOH/DCM (20 mL), filtered, adsorbed onto silica and then purified by silica chromatography eluting with 0-10% MeOH/DCM (1% NH4OH) to give the free base of the title compound as a yellow oil. LCMS/NMR consistent with the desired product.

후처리

  1. customto give an orange suspension
  2. stirringthe reaction was stirred for 3 h
  3. filtrationfiltered
  4. custompurified by silica chromatography
  5. washeluting with 0-10% MeOH/DCM (1% NH4OH)

출처 및 근거

ORD 기록
ord-8b5c958ffaab4c40ba6a240aaa0ae044
출처 데이터셋
uspto-grants-2013_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08389524B2

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