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Water → HCID 59410159, 화합물

HRID 391754
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HRID 391754 반응식
[Si:1]([O:18][CH2:19][CH2:20][C:21]1[C:22](=[O:53])[N:23]([C:27]2[C:32]([CH3:33])=[CH:31][C:30]([N:34]3[CH2:38][C@H:37]([CH2:39][N:40]4C(=O)C5C(=CC=CC=5)C4=O)[O:36][C:35]3=[O:51])=[CH:29][C:28]=2[CH3:52])[CH:24]=[CH:25][CH:26]=1)([C:14]([CH3:17])([CH3:16])[CH3:15])([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.CN.O.ClCCl>C(O)C>[NH2:40][CH2:39][C@@H:37]1[O:36][C:35](=[O:51])[N:34]([C:30]2[CH:29]=[C:28]([CH3:52])[C:27]([N:23]3[CH:24]=[CH:25][CH:26]=[C:21]([CH2:20][CH2:19][O:18][Si:1]([C:14]([CH3:15])([CH3:16])[CH3:17])([C:8]4[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=4)[C:2]4[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=4)[C:22]3=[O:53])=[C:32]([CH3:33])[CH:31]=2)[CH2:38]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 6329MethylamineHCID 6344DichloromethaneHCID 59410227HCID 59410227, 화합물

생성물 1

HCID 59410159HCID 59410159, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
52.5 °C

실험 절차

130 g (179 mmol) of the compound from Example 67A are dissolved in 650 ml of ethanol, 193 ml (2.68 mol) of a 40% strength aqueous methanamine solution are added and the mixture is heated at 50-55° C. for one hour. After cooling to room temperature, water and dichloromethane are added, the phases are separated and the organic phase is dried over sodium sulphate. After filtration, the mixture is evaporated to dryness under reduced pressure. The residue (117 g, 89% of theory) is reacted further without further purification.

후처리

  1. temperatureAfter cooling to room temperature
  2. customthe phases are separated
  3. dry with materialthe organic phase is dried over sodium sulphate
  4. filtrationAfter filtration
  5. customthe mixture is evaporated to dryness under reduced pressure
  6. customThe residue (117 g, 89% of theory) is reacted further without further purification

출처 및 근거

ORD 기록
ord-cc6156627c6f472fbb92c327b3454b08
출처 데이터셋
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08383822B2

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