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Ethanol → HCID 67040267, 화합물

HRID 605217
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인쇄 미리보기

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HRID 605217 반응식
[CH:1]1[C:13]2[CH:12]([CH2:14][O:15][C:16](=[O:45])[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:41])[NH:32][C:33]5[CH:34]=[N:35][C:36]([O:39][CH3:40])=[CH:37][CH:38]=5)=[CH:27][C:26]=4[N+:42]([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:45])[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:41])[NH:32][C:33]5[CH:34]=[N:35][C:36]([O:39][CH3:40])=[CH:37][CH:38]=5)=[CH:27][C:26]=4[NH2:42])=[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 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 702EthanolHCID 8028TetrahydrofuranHCID 25517Ammonium ChlorideHCID 67040155HCID 67040155, 화합물

생성물 1

HCID 67040267HCID 67040267, 화합물수율 92%

시약·촉매·용매 3

HCID 23925Iron촉매
HCID 962
Water
용매
HCID 8857Ethyl Acetate용매

반응 조건

온도
80 °C

실험 절차

The product of Example 201A (200 mg, 0.3233 mmol), ammonium chloride (113 mg, 2.118 mmol), and iron powder (111 mg, 1.988 mmol) in a mixture of water (3 mL), ethanol (6 mL) and tetrahydrofuran (6 mL) was heated at 80° C. under a nitrogen atmosphere for 75 minutes. The reaction was cooled to room temperature, diluted with ethyl acetate (100 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 a light beige solid (175 mg, 92%).

후처리

  1. temperatureThe reaction was cooled to room temperature
  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-e401686485ec4843b8f1dce219cd700b
출처 데이터셋
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07910595B2

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