Triethylamine → HCID 86733531, 화합물

HRID 1658815노트

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HRID 1658815 반응식
[CH3:1][O:2][C:3]([CH:5]([N:9]1[CH:12]([S:13][N:14]2[C:18](=[O:19])[CH2:17][CH2:16][C:15]2=[O:20])[CH:11]([NH:21][C:22](=[O:30])[CH2:23][C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)[C:10]1=[O:31])[C:6]([CH3:8])=[CH2:7])=[O:4].C(N(CC)CC)C>O1CCCC1>[CH3:1][O:2][C:3]([C:5]([N:9]1[CH:12]([S:13][N:14]2[C:18](=[O:19])[CH2:17][CH2:16][C:15]2=[O:20])[CH:11]([NH:21][C:22](=[O:30])[CH2:23][C:24]2[CH:25]=[CH:26][CH:27]=[CH:28][CH:29]=2)[C:10]1=[O:31])=[C:6]([CH3:8])[CH3:7])=[O:4]

참가 물질

4

반응물 2

HCID 8471TriethylamineHCID 86733532HCID 86733532, 화합물

생성물 1

HCID 86733531HCID 86733531, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
65 °C

실험 절차

A mixture of 2.25 g (5 mmoles) of 1-(1-methoxycarbonyl-2-methylprop-2-enyl)-3-phenylacetamido-4-succinimidothio-azetidin-2-one (prepared as described in Example 2) and 1.4 ml (10 mmoles) of triethylamine in 100 ml of tetrahydrofuran was stirred at 65°C for 25 minutes. The reaction mixture was evaporated, treated with 25 ml of ethyl acetate and evaporated once more. The residual foam was dissolved in 50 ml of ethyl acetate, treated with charcoal and concentrated to a small volume. The desired product crystallized upon cooling. There was obtained 1-(1-methoxycarbonyl-2-methylpropenyl)-3-phenylacetamido-4-succinimidothio-azetidin-2-one.

후처리

  1. customThe reaction mixture was evaporated
  2. additiontreated with 25 ml of ethyl acetate
  3. customevaporated once more
  4. dissolutionThe residual foam was dissolved in 50 ml of ethyl acetate
  5. additiontreated with charcoal
  6. concentrationconcentrated to a small volume
  7. customThe desired product crystallized
  8. temperatureupon cooling

출처 및 근거

ORD 기록
ord-2f7bcb2744d9483eb5b8b2fdfdac5709
출처 데이터셋
uspto-grants-1976_06
특허 번호
US03966738

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