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Cyanamide → 1H-Benzotriazole-1-carboximidamide--hydrogen chloride (1/1)

HRID 1192237
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HRID 1192237 반응식
[ClH:1].[NH:2]1[C:6]2[CH:7]=[CH:8][CH:9]=[CH:10][C:5]=2[N:4]=[N:3]1.[N:11]#[C:12][NH2:13]>CCOCC>[ClH:1].[N:2]1([C:12](=[NH:11])[NH2:13])[C:6]2[CH:7]=[CH:8][CH:9]=[CH:10][C:5]=2[N:4]=[N:3]1
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참가 물질

4

반응물 2

HCID 9864CyanamideHCID 178477914HCID 178477914, 화합물

생성물 1

HCID 534349021H-Benzotriazole-1-carboximidamide--hydrogen chloride (1/1)수율 71.2%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

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온도
80 °C

실험 절차

To a 5 mL CEM microwave reaction vessel, was charged benzotriazole HCl salt (0.5 g, 3.2 mmol) and cyanamide (0.16 g, 3.9 mmol). The vessel was sealed and heated at 80° C. for 1 minute under microwave irradiation (CEM Discovery™). After this time, TLC analysis showed no starting material remaining so the mixture was diluted with ether. The precipitate was collected by filtration and washed with ether and dried under vacuum to afford the titled product as a white solid (0.45 g, 71% yield). 1H NMR (400 MHz, d6-DMSO) δ: 10.14 (4H, s), 8.31 (1H, m), 8.05 (1H, m), 7.90 (1H, m), 7.67 ('H, m). MS m/z: 162.13 [M+H]+.

후처리

  1. customTo a 5 mL CEM microwave reaction vessel
  2. customThe vessel was sealed
  3. filtrationThe precipitate was collected by filtration
  4. washwashed with ether
  5. customdried under vacuum

출처 및 근거

ORD 기록
ord-b8e131378a704e219eeafe209a30c357
출처 데이터셋
uspto-grants-2014_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08680139B2

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