Acetic Acid → 7-Bromo-1,2,4,5-tetrahydro-pyrido[2,3-e][1,4]diazepin-3-one

HRID 2097107노트

반응식

HRID 2097107 반응식
[NH:1]1[C:7]2[N:8]=[CH:9][CH:10]=[CH:11][C:6]=2[CH2:5][NH:4][C:3](=[O:12])[CH2:2]1.C(O)(=O)C.[Br:17]Br>CCCCCC>[Br:17][C:10]1[CH:9]=[N:8][C:7]2[NH:1][CH2:2][C:3](=[O:12])[NH:4][CH2:5][C:6]=2[CH:11]=1

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 24408BromineHCID 592775691H,2H,3H,4H,5H-pyrido[2,3-e][1,4]diazepin-3-one

생성물 1

HCID 592776207-Bromo-1,2,4,5-tetrahydro-pyrido[2,3-e][1,4]diazepin-3-one

시약·촉매·용매 1

HCID 8058Hexane용매

실험 절차

1,2,4,5-Tetrahydro-pyrido[2,3-e][1,4]diazepin-3-one (164 mg, 1.0 mmol) was dissolved into acetic acid (1 mL). Bromine (160 mg, 1.0 mmol) was added dropwise at room temperature and the solution was stirred overnight. Hexane (5 mL) was added and the orange precipitate was filtered and dried in vacuo. The title compound was isolated as an orange solid (190 mg, 78%). 1H NMR (300 MHz, DMSO-d6) δ 8.26 (t, J=5.7 Hz, 1H), 8.06 (d, J=2.1 Hz, 1H), 7.81 (d, J=2.1 Hz, 1H), 4.35 (d, J=5.7 Hz, 2H), 4.08 (s, 2H).

후처리

  1. filtrationthe orange precipitate was filtered
  2. customdried in vacuo

출처 및 근거

ORD 기록
ord-57fe8c1fda42440d85d65c635be9f383
출처 데이터셋
uspto-grants-2013_05
특허 번호
US08450307B2

반응 노트

불러오는 중…