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Sodium Bicarbonate → HCID 58782546, 화합물

HRID 1374476
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HRID 1374476 반응식
[CH3:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH3:8])[C:3]=1[C:9]([N:11]1[CH2:18][CH:17]2[CH:13]([CH2:14][NH:15][CH2:16]2)[CH2:12]1)=[O:10].O=[C:20]([CH3:37])[CH2:21][CH:22]([NH:29][C:30]([CH:32]1[CH2:36][CH2:35][CH2:34][CH2:33]1)=[O:31])[C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1.[BH-](OC(C)=O)(OC(C)=O)OC(C)=O.[Na+].C([O-])(O)=O.[Na+]>C(Cl)Cl.C1COCC1.CC(C)[O-].CC(C)[O-].CC(C)[O-].CC(C)[O-].[Ti+4].O>[CH3:8][C:4]1[CH:5]=[CH:6][CH:7]=[C:2]([CH3:1])[C:3]=1[C:9]([N:11]1[CH2:18][CH:17]2[CH2:16][N:15]([CH:20]([CH3:37])[CH2:21][C@H:22]([NH:29][C:30]([CH:32]3[CH2:36][CH2:35][CH2:34][CH2:33]3)=[O:31])[C:23]3[CH:24]=[CH:25][CH:26]=[CH:27][CH:28]=3)[CH2:14][CH:13]2[CH2:12]1)=[O:10]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 4

HCID 516892Sodium BicarbonateHCID 5049666Sodium triacetoxyborohydrideHCID 21076152HCID 21076152, 화합물HCID 69436264HCID 69436264, 화합물

생성물 1

HCID 58782546HCID 58782546, 화합물

시약·촉매·용매 4

HCID 11026Titanium isopropoxide
촉매
HCID 962Water용매
HCID 6344Dichloromethane용매
HCID 8028Tetrahydrofuran용매

실험 절차

step 5—To a solution of (2,6-dimethyl-phenyl)-(hexahydro-pyrrolo[3,4-c]pyrrol-2-yl)-methanone (66, 0.12 g, 0.52 mmol) in DCM (7 mL) and THF (7 mL) was added cyclopentanecarboxylic acid (3-oxo-1-phenyl-butyl)-amide (85d, 0.15 g, 0.57 mmol). Titanium tetraisopropoxide (0.34 mL, 1.15 mmol) was added to the mixture. After 30 min NaBH(OAc)3 (0.16 g, 0.78 mmol) was added and the mixture stirred at RT for 4 h. Saturated NaHCO3 was added to the mixture and it was stirred for 10 min. The mixture was extracted with DCM and the organic layer was dried (MgSO4), filtered and evaporated. The crude product was purified by SiO2 chromatography on silica gel eluting with DCM:MeOH:NH4OH (150:10:1) to afford I-75: ms (ES+) m/z 488 (M+H); Anal. (C31H41N3O2.0.3M H2O)C; calcd, 75.51; found 75.53; H; calcd, 8.50; found, 8.29; N; calcd, 8.52; found, 8.53.

후처리

  1. stirringwas stirred for 10 min
  2. extractionThe mixture was extracted with DCM
  3. dry with materialthe organic layer was dried (MgSO4)
  4. filtrationfiltered
  5. customevaporated
  6. customThe crude product was purified by SiO2 chromatography on silica gel eluting with DCM:MeOH:NH4OH (150:10:1)
  7. customto afford I-75: ms (ES+) m/z 488 (M+H)

출처 및 근거

ORD 기록
ord-ce411700ffc64cb285357274e664be28
출처 데이터셋
uspto-grants-2007_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07164019B2

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