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Water → HCID 57406041, 화합물

HRID 1910464
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HRID 1910464 반응식
[C:1](#[N:7])[CH2:2][CH2:3][CH2:4][C:5]#[N:6].N[NH:9][C:10]([NH2:12])=[S:11].O.[OH-].[Na+]>C(O)(C(F)(F)F)=O>[CH2:2]([C:1]1[S:11][C:10]([NH2:12])=[N:9][N:7]=1)[CH2:3][CH2:4][C:5]1[S:11][C:10]([NH2:12])=[N:9][N:6]=1
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참가 물질

6

반응물 4

HCID 962WaterHCID 10994GlutaronitrileHCID 14798Sodium HydroxideHCID 2723789Thiosemicarbazide

생성물 1

HCID 57406041HCID 57406041, 화합물수율 106.6%

시약·촉매·용매 1

HCID 6422Trifluoroacetic acid용매

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온도
85 °C

실험 절차

A mixture of glutaronitrile (5.00 g, 53.13 mmol) and thiosemicarbazide (9.68 g, 106.26 mmol) in TFA (50 mL) was heated at 85° C. for 4 h. The reaction was cooled to room temperature and poured into a mixture of ice and water. Sodium hydroxide pellets were added to the mixture until it was basic (pH 14). The white precipitate was collected by suction filtration, rinsed with water and dried to provide 5,5′-(propane-1,3-diyl)-bis(1,3,4-thiadiazol-2-amine) (1004, 13.72 g). 1H NMR (300 MHz, DMSO-d6) δ 7.06-7.03 (s, 4H), 2.87 (t, J=7.5 Hz, 4H), 2.02-1.95 (m, 2H).

후처리

  1. temperatureThe reaction was cooled to room temperature
  2. filtrationThe white precipitate was collected by suction filtration
  3. washrinsed with water
  4. customdried

출처 및 근거

ORD 기록
ord-8911f32819d14727a87facc77d5c305c
출처 데이터셋
uspto-grants-2013_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08604016B2

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