Triethylamine → HCID 67391050, 화합물

HRID 906442노트

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HRID 906442 반응식
[N:1]1([C:8]([O:10][C:11]([CH3:14])([CH3:13])[CH3:12])=[O:9])[CH2:7][CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.C(N(CC)CC)C.[Br:22][C:23]1[CH:24]=[C:25]2[C:30](=[CH:31][CH:32]=1)[C:29](=[O:33])[NH:28][CH:27]=[C:26]2[S:34](Cl)(=[O:36])=[O:35]>C1COCC1>[Br:22][C:23]1[CH:24]=[C:25]2[C:30](=[CH:31][CH:32]=1)[C:29](=[O:33])[NH:28][CH:27]=[C:26]2[S:34]([N:4]1[CH2:5][CH2:6][CH2:7][N:1]([C:8]([O:10][C:11]([CH3:14])([CH3:13])[CH3:12])=[O:9])[CH2:2][CH2:3]1)(=[O:36])=[O:35]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 2756058Tert-butyl 1,4-diazepane-1-carboxylateHCID 574399006-Bromo-1-oxo-1,2-dihydroisoquinoline-4-sulfonyl chloride

생성물 1

HCID 67391050HCID 67391050, 화합물수율 72.8%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

To a solution of tert-butyl 1,4-diazepane-1-carboxylate (0.621 g) and triethylamine (0.864 mL) in THF (12 mL) was added dropwise a solution of 6-bromo-1-oxo-1,2-dihydroisoquinoline-4-sulfonyl chloride (Example 46a, 1 g) in THF (20 mL). The reaction was stirred at room temperature for 20 min. The resulting solution was concentrated under reduced pressure, acidified with 2 M HCl, and extracted into ethyl acetate. The combined organics were dried (MgSO4), filtered and evaporated under reduced pressure to give the subtitle compound (1.097 g) that was used without further purification.

후처리

  1. concentrationThe resulting solution was concentrated under reduced pressure
  2. extractionextracted into ethyl acetate
  3. dry with materialThe combined organics were dried (MgSO4)
  4. filtrationfiltered
  5. customevaporated under reduced pressure

출처 및 근거

ORD 기록
ord-d40b05ca164147fabfb0fb1ea4d392dc
출처 데이터셋
uspto-grants-2011_09
특허 번호
US08012980B2

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