Water → 5-(2-((2-(5-Amino-1,3,4-thiadiazol-2-yl)ethyl)amino)ethyl)-1,3,4-thiadiazol-2-amine

HRID 538089

반응식

HRID 538089 반응식
[NH:1]([CH2:6][CH2:7][C:8]#[N:9])[CH2:2][CH2:3][C:4]#[N:5].N[NH:11][C:12]([NH2:14])=[S:13].O.[OH-].[Na+]>C(O)(C(F)(F)F)=O>[NH2:11][C:12]1[S:13][C:4]([CH2:3][CH2:2][NH:1][CH2:6][CH2:7][C:8]2[S:13][C:12]([NH2:14])=[N:11][N:9]=2)=[N:5][N:14]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 81493,3'-IminodipropionitrileHCID 14798Sodium HydroxideHCID 2723789Thiosemicarbazide

생성물 1

HCID 39507595-(2-((2-(5-Amino-1,3,4-thiadiazol-2-yl)ethyl)amino)ethyl)-1,3,4-thiadiazol-2-amine수율 44.5%

시약·촉매·용매 1

HCID 6422Trifluoroacetic acid용매

실험 절차

A mixture of 3,3′-iminodipropionitrile (1.50 g, 12.18 mmol) and thiosemicarbazide (2.22 g, 24.36 mmol) in TFA (10 mL) was heated at 85 for 4.5 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-(2-((2-(5-amino-1,3,4-thiadiazol-2-yl)ethyl)amino)ethyl)-1,3,4-thiadiazol-2-amine (1005, 1.47 g). 1H NMR (300 MHz, DMSO-d6) δ 6.95 (s, 4H), 2.90 (d, J=6.0 Hz, 4H), 2.83 (d, J=6.3 Hz, 4H).

후처리

  1. temperaturewas heated at 85 for 4.5 h
  2. filtrationThe white precipitate was collected by suction filtration
  3. washrinsed with water
  4. customdried

출처 및 근거

ORD 기록
ord-d731ef372b504249a8182a6dcfe22a2c
출처 데이터셋
uspto-grants-2014_10
특허 번호
US08865718B2

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