Benzaldehyde → Bis(4-(2-benzalaminoethyl)piperazine-1-thiocarbonyl) Disulfane

HRID 1032000노트

반응식

HRID 1032000 반응식
[CH:1](=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[NH2:9][CH2:10][CH2:11][N:12]1[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]1.[C:18](=[S:20])=[S:19]>[C-]#N.[C-]#N.[C-]#N.[C-]#N.[C-]#N.[C-]#N.[K+].[K+].[K+].[Fe+3].C(N(CC)CC)C.C(O)C.O>[CH:1](=[N:9][CH2:10][CH2:11][N:12]1[CH2:17][CH2:16][N:15]([C:18]([S:20][S:20][C:18]([N:15]2[CH2:16][CH2:17][N:12]([CH2:11][CH2:10][N:9]=[CH:1][C:2]3[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=3)[CH2:13][CH2:14]2)=[S:19])=[S:19])[CH2:14][CH2:13]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

8

반응물 3

HCID 240BenzaldehydeHCID 6348Carbon DisulfideHCID 8795Aminoethylpiperazine

생성물 1

HCID 86744207Bis(4-(2-benzalaminoethyl)piperazine-1-thiocarbonyl) Disulfane

시약·촉매·용매 4

HCID 26250Potassium ferricyanide촉매HCID 702Ethanol용매2회HCID 962Water용매2회HCID 8471Triethylamine용매

실험 절차

10.6 parts of benzaldehyde are added to a solution of 12.9 parts of 1-(2-aminoethyl)piperazine in 24 parts of water and 24 parts of ethanol. 7.6 parts of carbon disulfide are then slowly added dropwise with ice cooling, whereby a precipitate forms. This is again dissolved after dilution with 100 parts each of water and of ethanol by addition of 10.1 parts of triethylamine and oxidized with 33 parts with potassium hexacyanoferrate(III). The product that now precipitates is filtered, washed repeatedly with water and finally with methanol, and dried at 30° C. in vacuum. Obtained are 26 parts of a substance with 56.4% C, 6.3% H, 14.5% N, and 21.5% S (calculated: 57.5% C, 6.2% H, 14.4% N, 21.9% S), which corresponds to the title compound of this Example according to IR and 1H-NMR.

후처리

  1. customThe product that now precipitates
  2. filtrationis filtered
  3. washwashed repeatedly with water and finally with methanol
  4. customdried at 30° C. in vacuum
  5. customObtained

출처 및 근거

ORD 기록
ord-d248eaf8c8f946bf876c71d1d6e3a01d
출처 데이터셋
uspto-grants-1990_09
특허 번호
US04956433

반응 노트

불러오는 중…