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1,2-Dichloroethane → HCID 58537189, 화합물

HRID 1804503
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HRID 1804503 반응식
[CH2:1]([C:5]1[O:9][N:8]=[C:7]([C:10]([OH:12])=O)[C:6]=1[CH2:13][CH2:14][CH3:15])[CH:2]([CH3:4])[CH3:3].[CH2:16]([C:20]1[C:21]([C:28]([OH:30])=O)=[N:22][O:23][C:24]=1[CH2:25][CH2:26][CH3:27])[CH:17]([CH3:19])[CH3:18].O/[N:32]=[C:33](/[C:35]1[CH:52]=[CH:51][C:38]([CH2:39][N:40]2[CH2:43][CH:42]([C:44]([O:46][C:47]([CH3:50])([CH3:49])[CH3:48])=[O:45])[CH2:41]2)=[CH:37][CH:36]=1)\[NH2:34].C1C=CC2N(O)N=NC=2C=1.C(N(C(C)C)CC)(C)C.C(Cl)CCl>CN(C=O)C>[CH2:1]([C:5]1[O:9][N:8]=[C:7]([C:10]2[O:12][N:34]=[C:33]([C:35]3[CH:36]=[CH:37][C:38]([CH2:39][N:40]4[CH2:41][CH:42]([C:44]([O:46][C:47]([CH3:48])([CH3:50])[CH3:49])=[O:45])[CH2:43]4)=[CH:51][CH:52]=3)[N:32]=2)[C:6]=1[CH2:13][CH2:14][CH3:15])[CH:2]([CH3:3])[CH3:4].[CH2:16]([C:20]1[C:21]([C:28]2[O:30][N:34]=[C:33]([C:35]3[CH:36]=[CH:37][C:38]([CH2:39][N:40]4[CH2:41][CH:42]([C:44]([O:46][C:47]([CH3:48])([CH3:50])[CH3:49])=[O:45])[CH2:43]4)=[CH:51][CH:52]=3)[N:32]=2)=[N:22][O:23][C:24]=1[CH2:25][CH2:26][CH3:27])[CH:17]([CH3:18])[CH3:19]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 6

HCID 111,2-DichloroethaneHCID 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 58504340HCID 58504340, 화합물HCID 58537221HCID 58537221, 화합물HCID 58537233HCID 58537233, 화합물

생성물 2

HCID 58537189
HCID 58537189, 화합물
수율 66.6%
HCID 58537195HCID 58537195, 화합물수율 66.6%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

A mixture of 5-isobutyl-4-propylisoxazole-3-carboxylic acid, and 4-isobutyl-5-propylisoxazole-3-carboxylic acid (42.26 mg, 0.2 mmol), (Z)-tert-butyl 1-(4-(N′-hydroxycarbamimidoyl)benzyl)azetidine-3-carboxylate (61.1 mg, 0.200 mmol), HOBt (38.3 mg, 0.250 mmol), diisopropylethylamine (0.070 mL, 0.400 mmol) and EDC (47.9 mg, 0.250 mmol) in DMF (1 mL) was stirred at rt for 18 hr. DMF (1 mL) was added and the reaction mixture was warmed to 50° C. for 8 hr. The reaction mixture was partitioned between EtOAc (30 ml) and saturated sodium bicarbonate solution (30 ml). The organic layer was washed with water (2×30 ml) and brine (30 ml). After drying (MgSO4) and filtration, the organic layer was concentrated to afford an oil that was chromatographed on a 4 gm Isco silica gel cartridge, eluting with a 0-100% EtOAc/Hex gradient. The pure fractions were concentrated to afford a mixture of tert-butyl 1-(4-(5-(5-isobutyl-4-propylisoxazol-3-yl)-1,2,4-oxadiazol-3-yl)benzyl)azetidine-3-carboxylate (32 mg, 0.067 mmol, 66.6% yield) and tert-butyl 1-(4-(5-(4-isobutyl-5-propylisoxazol-3-yl)-1,2,4-oxadiazol-3-yl)benzyl)azetidine-3-carboxylate (32 mg, 0.067 mmol, 66.6% yield) as a colorless oil. HPLC retention time=1.89 minutes (YMC Combi 4.6×30 mm S-5 ODS column) eluting with 10-90% aqueous methanol+0.1 TFA a 2 minute gradient.

후처리

  1. temperaturethe reaction mixture was warmed to 50° C. for 8 hr
  2. customThe reaction mixture was partitioned between EtOAc (30 ml) and saturated sodium bicarbonate solution (30 ml)
  3. washThe organic layer was washed with water (2×30 ml) and brine (30 ml)
  4. customAfter drying
  5. filtration(MgSO4) and filtration
  6. concentrationthe organic layer was concentrated
  7. customto afford an oil that
  8. customwas chromatographed on a 4 gm Isco silica gel cartridge
  9. washeluting with a 0-100% EtOAc/Hex gradient
  10. concentrationThe pure fractions were concentrated
  11. customto afford

출처 및 근거

ORD 기록
ord-9b36985d526f45f89c689d54dd4891b3
출처 데이터셋
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08354398B2

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