N-bromobutanimide → HCID 67142870, 화합물

HRID 1270291노트

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HRID 1270291 반응식
[C:1]([NH:4][C:5]1[C:6]2[CH:13]=[CH:12][N:11]([C@@H:14]3[O:26][C@H:25]([CH2:27][O:28][C:29](=[O:31])[CH3:30])[C@@H:20]([O:21][C:22](=[O:24])[CH3:23])[C@@:15]3([CH3:32])[O:16][C:17](=[O:19])[CH3:18])[C:7]=2[N:8]=[CH:9][N:10]=1)(=[O:3])[CH3:2].[Br:33]N1C(=O)CCC1=O>CN(C=O)C>[C:1]([NH:4][C:5]1[C:6]2[C:13]([Br:33])=[CH:12][N:11]([C@@H:14]3[O:26][C@H:25]([CH2:27][O:28][C:29](=[O:31])[CH3:30])[C@@H:20]([O:21][C:22](=[O:24])[CH3:23])[C@@:15]3([CH3:32])[O:16][C:17](=[O:19])[CH3:18])[C:7]=2[N:8]=[CH:9][N:10]=1)(=[O:3])[CH3:2]

참가 물질

4

반응물 2

HCID 67184N-bromobutanimideHCID 67142229HCID 67142229, 화합물

생성물 1

HCID 67142870HCID 67142870, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

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온도
0 °C

실험 절차

To a pre-cooled (0° C.) solution of the compound from Step A (460 mg, 1.00 mmol) in DMF is added N-bromosuccinimide (178 mg, 1.0 mmol) in DMF. The resulting solution is stirred at 0° C. for 30 min then at room temperature for another 30 min. The reaction is quenched by addition of methanol and evaporated in vacuo. The resulting crude mixture is purified on silica gel using ethyl acetate/hexane as the eluent. Fractions containing the desired product are pooled and evaporated in vacuo to give the desired product.

후처리

  1. waitat room temperature for another 30 min
  2. customThe reaction is quenched by addition of methanol
  3. customevaporated in vacuo
  4. customThe resulting crude mixture is purified on silica gel
  5. additionFractions containing the desired product
  6. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-247d5fc0f643489092e8b2706db98e25
출처 데이터셋
uspto-grants-2007_04
특허 번호
US07202224B2

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