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Ethanol → HCID 67040715, 화합물

HRID 883942
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HRID 883942 반응식
[CH:1]1[C:13]2[CH:12]([CH2:14][O:15][C:16](=[O:44])[NH:17][C:18]3[CH:23]=[CH:22][C:21]([S:24][C:25]4[CH:30]=[CH:29][C:28]([C:31](=[O:40])[NH:32][C:33]5[CH:38]=[CH:37][C:36]([Cl:39])=[CH:35][N:34]=5)=[CH:27][C:26]=4[N+:41]([O-])=O)=[CH:20][CH:19]=3)[C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5]=2[CH:4]=[CH:3][CH:2]=1.[Cl-].[NH4+].C(O)C.O1CCCC1>O.C(OCC)(=O)C.[Fe]>[CH:1]1[C:13]2[CH:12]([CH2:14][O:15][C:16](=[O:44])[NH:17][C:18]3[CH:19]=[CH:20][C:21]([S:24][C:25]4[CH:30]=[CH:29][C:28]([C:31](=[O:40])[NH:32][C:33]5[CH:38]=[CH:37][C:36]([Cl:39])=[CH:35][N:34]=5)=[CH:27][C:26]=4[NH2:41])=[CH:22][CH:23]=3)[C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5]=2[CH:4]=[CH:3][CH:2]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 702EthanolHCID 8028TetrahydrofuranHCID 25517Ammonium ChlorideHCID 67040866HCID 67040866, 화합물

생성물 1

HCID 67040715HCID 67040715, 화합물수율 91%

시약·촉매·용매 3

HCID 23925Iron촉매
HCID 962
Water
용매
HCID 8857Ethyl Acetate용매

실험 절차

The product of Example 52D (371 mg, 0.5954 mmol), ammonium chloride (208.6 mg, 3.900 mmol), and iron powder (204.5 mg, 3.662 mmol) in a mixture of water (6 mL), ethanol (12 mL) and tetrahydrofuran (12 mL) was heated at 90° under a nitrogen atmosphere for 3 hours. The reaction was cooled to room temperature, diluted with ethyl acetate (200 mL), and washed with water (2×50 mL) and brine (50 mL). The organic was dried over anhydrous sodium sulfate, filtered, and concentrated by rotary evaporation in vacuo to give the product as an off-white solid (321 mg, 91%).

후처리

  1. temperaturewas heated at 90° under a nitrogen atmosphere for 3 hours
  2. washwashed with water (2×50 mL) and brine (50 mL)
  3. dry with materialThe organic was dried over anhydrous sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated by rotary evaporation in vacuo

출처 및 근거

ORD 기록
ord-0a838de089e142bea3ea10f365ddd540
출처 데이터셋
uspto-grants-2012_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08236950B2

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