Dimethylformamide → HCID 59216558, 화합물

HRID 386488

반응식

HRID 386488 반응식
Cl[C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[CH:5]=[C:4]([Cl:12])[N:3]=1.[NH:13]1[CH2:18][CH2:17][CH:16]([NH:19][C:20](=[O:26])[O:21][CH2:22][CH:23]([CH3:25])[CH3:24])[CH2:15][CH2:14]1.CCN(CC)CC.CN(C=O)C>O>[Cl:12][C:4]1[N:3]=[C:2]([N:13]2[CH2:14][CH2:15][CH:16]([NH:19][C:20](=[O:26])[O:21][CH2:22][CH:23]([CH3:24])[CH3:25])[CH2:17][CH2:18]2)[C:11]2[C:6]([CH:5]=1)=[CH:7][CH:8]=[CH:9][CH:10]=2

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 8471TriethylamineHCID 2986251,3-DichloroisoquinolineHCID 15676964HCID 15676964, 화합물

생성물 1

HCID 59216558HCID 59216558, 화합물

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
160 °C

실험 절차

A mixture of 1,3-dichloroisoquinoline (0.16 g, 0.78 mmol), isobutyl piperidin-4-ylcarbamate (0.16 g, 0.78 mmol), Et3N (0.11 mL, 0.78 mmol), and DMF (0.5 mL) was sealed in a microwave vessel and heated by microwave irradiation at 160° C. for three minutes. The reaction was cooled to room temperature, diluted with water, and extracted with CH2Cl2. The combined extracts were washed with water, dried over Na2SO4, and concentrated under reduced pressure to yield isobutyl 1-(3-chloroisoquinolin-1-yl)piperidin-4-ylcarbamate. LC/MS: m/z 362.2 (M+H)+ at 3.98 min (10%-99% CH3CN (0.035% TFA)/H2O (0.05% TFA)).

후처리

  1. customwas sealed in a microwave vessel
  2. temperatureThe reaction was cooled to room temperature
  3. extractionextracted with CH2Cl2
  4. washThe combined extracts were washed with water
  5. dry with materialdried over Na2SO4
  6. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-12e5f6bc9b594acc8a4aca313eb831ae
출처 데이터셋
uspto-grants-2013_02
특허 번호
US08372843B2

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