Formaldehyde → Benzotriazol-1-ylmethyl-(2-thiophen-2-yl-ethyl)-amine

HRID 1676506노트

반응식

HRID 1676506 반응식
[NH:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[N:3]=[N:2]1.[S:10]1[CH:14]=[CH:13][CH:12]=[C:11]1[CH2:15][CH2:16][NH2:17].[CH2:18]=O>CCOCC>[N:1]1([CH2:18][NH:17][CH2:16][CH2:15][C:11]2[S:10][CH:14]=[CH:13][CH:12]=2)[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[N:3]=[N:2]1

참가 물질

5

반응물 3

HCID 712FormaldehydeHCID 116521ThiopheneethanamineHCID 178418385HCID 178418385, 화합물

생성물 1

HCID 86637495Benzotriazol-1-ylmethyl-(2-thiophen-2-yl-ethyl)-amine수율 100.6%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

To a mixture of 12 g (0.1 mole) benzotriazole and 13 g (0.1 mole) of 2-thiophen-2-yl-ethylamine in 500 mL of ether was added dropwise 7.4 mL (0.1 mole) of 37% aqueous formaldehyde. The reaction mixture was stirred at room temperature overnight. The solution was dried over calcium chloride, filtered and concentrated under pressure. Hexane was added to the residue cooled in an ice bath and the resulting solid was collected by filtration, washing with hexane and then dried to give 26.0 g of benzotriazol-1-ylmethyl-(2-thiophen-2-yl-ethyl)-amine as a light yellow oil (100%).

후처리

  1. dry with materialThe solution was dried over calcium chloride
  2. filtrationfiltered
  3. concentrationconcentrated under pressure
  4. additionHexane was added to the residue
  5. temperaturecooled in an ice bath
  6. filtrationthe resulting solid was collected by filtration
  7. washwashing with hexane
  8. customdried

출처 및 근거

ORD 기록
ord-dd856bbe421f422e85ec2134d5f4d93d
출처 데이터셋
uspto-grants-2011_08
특허 번호
US08003785B2

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