Triethylamine → HCID 16658527, 화합물

HRID 2289823노트

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HRID 2289823 반응식
[Cl:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[C:9]([S:12](Cl)(=[O:14])=[O:13])[CH:10]=2)[C:5]([Cl:16])=[CH:4][N:3]=1.[NH:17]1[CH2:22][CH2:21][CH2:20][CH2:19][C@@H:18]1[C:23]([O:25][C:26]([CH3:29])([CH3:28])[CH3:27])=[O:24].C(N(CC)CC)C>C(Cl)Cl>[Cl:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[C:9]([S:12]([N:17]3[CH2:22][CH2:21][CH2:20][CH2:19][C@@H:18]3[C:23]([O:25][C:26]([CH3:29])([CH3:28])[CH3:27])=[O:24])(=[O:14])=[O:13])[CH:10]=2)[C:5]([Cl:16])=[CH:4][N:3]=1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 166582941,4-Dichloroisoquinoline-7-sulfonyl chlorideHCID 21969834tert-butyl (2R)-piperidine-2-carboxylate

생성물 1

HCID 16658527HCID 16658527, 화합물수율 78.3%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

1,4-Dichloro-7-isoquinolinylsulphonyl chloride (245 mg, 0.83 mmol) was added to a solution of tert-butyl 2(R)-piperidine carboxylate (153 mg, 0.83 mmol) and triethylamine (170 μl, 1.22 mmol) in CH2Cl2 (15 ml), and the reaction stirred at room temperature for 18 h. The solution was diluted with CH2Cl2, washed with 2M hydrochloric acid, saturated Na2CO3 solution and then brine, dried (MgSO4), and evaporated in vacuo. The residual oil was purified by column chromatography upon silica gel using an elution gradient of pentane-EtOAc (100:0 to 90:10), to give tert-butyl (2R)-1-[(1,4-dichloro-7-isoquinolinyl)sulphonyl]-2-piperidinecarboxylate, (290 mg, 0.65 mmol) as a colourless film.

후처리

  1. washwashed with 2M hydrochloric acid, saturated Na2CO3 solution
  2. dry with materialbrine, dried (MgSO4)
  3. customevaporated in vacuo
  4. customThe residual oil was purified by column chromatography upon silica gel using an elution gradient of pentane-EtOAc (100:0 to 90:10)

출처 및 근거

ORD 기록
ord-d4f84f249714427d9a75158b0c72eb88
출처 데이터셋
uspto-grants-2000_07
특허 번호
US06093731

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