Diethyl Ether → 4-dimethylaminomethylene-7-iodo-3,4-dihydro-1H-benzo[b]azepine-2,5-dione

HRID 2373360노트

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HRID 2373360 반응식
[I:1][C:2]1[CH:14]=[CH:13][C:5]2[NH:6][C:7](=[O:12])[CH2:8][CH2:9][C:10](=[O:11])[C:4]=2[CH:3]=1.CO[CH:17](OC)[N:18]([CH3:20])[CH3:19].CCOCC>C1COCC1>[CH3:17][N:18]([CH:20]=[C:9]1[CH2:8][C:7](=[O:12])[NH:6][C:5]2[CH:13]=[CH:14][C:2]([I:1])=[CH:3][C:4]=2[C:10]1=[O:11])[CH3:19]

참가 물질

5

반응물 3

HCID 3283Diethyl EtherHCID 78373Dimethylformamide dimethyl acetalHCID 120121827-Iodo-3,4-dihydro-1H-benzo[b]azepine-2,5-dione

생성물 1

HCID 669350664-dimethylaminomethylene-7-iodo-3,4-dihydro-1H-benzo[b]azepine-2,5-dione

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
70 °C

실험 절차

To a solution of 7-iodo-3,4-dihydro-1H-benzo[b]azepine-2,5-dione (iv-a) (1.67 g, 5.54 mmol) in THF (15 mL) was added dimethylformamide dimethylacetal (4.0 mL, 27.7 mmol) and the reaction mixture heated to 70° C. for 1 h. The reaction mixture was cooled to 22° C., treated with Et2O (50 mL), and the resulting precipitate filtered and dried in vacuo to give v-a (1.64 g, 83%) as a brown powder: MS m/z═357 (M+H).

후처리

  1. temperatureThe reaction mixture was cooled to 22° C.
  2. filtrationthe resulting precipitate filtered
  3. customdried in vacuo
  4. customto give v-a (1.64 g, 83%) as a brown powder

출처 및 근거

ORD 기록
ord-8556e4fbd71f4505b78806652abb3204
출처 데이터셋
uspto-grants-2008_12
특허 번호
US07459448B2

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