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Ethanol → HCID 67040841, 화합물

HRID 605184
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HRID 605184 반응식
[CH:1]1[C:13]2[CH:12]([CH2:14][O:15][C:16](=[O:46])[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:42])[NH:32][C:33]5[S:34][C:35]([C:38]([F:41])([F:40])[F:39])=[N:36][N:37]=5)=[CH:27][C:26]=4[N+:43]([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:10]1[C:11]2[CH:12]([CH2:14][O:15][C:16](=[O:46])[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:42])[NH:32][C:33]5[S:34][C:35]([C:38]([F:39])([F:41])[F:40])=[N:36][N:37]=5)=[CH:27][C:26]=4[NH2:43])=[CH:22][CH:23]=3)[C:13]3[C:5](=[CH:4][CH:3]=[CH:2][CH:1]=3)[C:6]=2[CH:7]=[CH:8][CH:9]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 702EthanolHCID 8028TetrahydrofuranHCID 25517Ammonium ChlorideHCID 67040654HCID 67040654, 화합물

생성물 1

HCID 67040841HCID 67040841, 화합물

시약·촉매·용매 3

HCID 23925Iron촉매
HCID 962
Water
용매
HCID 8857Ethyl Acetate용매

반응 조건

온도
90 °C

실험 절차

The product of Example 154A (307 mg, 0.463 mmol), ammonium chloride (162 mg, 3.03 mmol), and iron powder (159 mg, 2.845 mmol) in a mixture of water (3 mL), ethanol (6 mL) and tetrahydrofuran (6 mL) was heated at 90° C. under a nitrogen atmosphere for 1 hour. The reaction was cooled to room temperature, diluted with ethyl acetate (100 mL), and washed with water (3×50 mL) and brine (50 mL). The organic phase was dried over anhydrous sodium sulfate, filtered, and concentrated by rotary evaporation in vacuo to give the product as a light yellow solid (224 mg, 76

후처리

  1. temperatureThe reaction was cooled to room temperature
  2. washwashed with water (3×50 mL) and brine (50 mL)
  3. dry with materialThe organic phase was dried over anhydrous sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated by rotary evaporation in vacuo

출처 및 근거

ORD 기록
ord-2cf2bcfb970c4343990cc2d208b4758c
출처 데이터셋
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07910595B2

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