Ammonium Hydroxide → 3-Amino-4-n-butoxy-3-cyclobutene-1,2-dione

HRID 1651339

반응식

HRID 1651339 반응식
[CH2:1]([O:5][C:6]1[C:9](=[O:10])[C:8](=[O:11])[C:7]=1OCCCC)[CH2:2][CH2:3][CH3:4].[OH-].[NH4+:18]>O1CCCC1.CO>[NH2:18][C:7]1[C:8](=[O:11])[C:9](=[O:10])[C:6]=1[O:5][CH2:1][CH2:2][CH2:3][CH3:4]

참가 물질

5

반응물 2

HCID 14923Ammonium HydroxideHCID 65108Dibutyl squarate

생성물 1

HCID 145450343-Amino-4-n-butoxy-3-cyclobutene-1,2-dione

시약·촉매·용매 2

HCID 887Methanol용매HCID 8028Tetrahydrofuran용매2회

반응 조건

온도
5 °C

실험 절차

Preparation A: A solution of 1,2-dibutoxy-1-cyclobutene-3,4-dione (6.09, 0.027 mole) in 40 mL of tetrahydrofuran was cooled to 5° C. in an ice-water bath and treated dropwise over a period of 9 minutes with a solution of 1.8 mL of concentrated ammonium hydroxide in a mixture of 8 mL of tetrahydrofuran and 1 mL of methanol. After stirring at 5° C. for 30 minutes and at ambient temperature for 90 minutes the mixture was concentrated under reduced pressure to a slurry. A small amount of Skellysolve B was added and the product was collected by filtration after 16 hours of standing at 0° C. to give 3.26 g of the title compound. A sample (8.54 g) was partly dissolved in acetone, filtered and cooled to give 4.51 g of purified title compound; mp=165.5°-168° C. (clear melt).

후처리

  1. concentrationwas concentrated under reduced pressure to a slurry
  2. additionA small amount of Skellysolve B was added
  3. filtrationthe product was collected by filtration after 16 hours
  4. customof standing at 0° C.

출처 및 근거

ORD 기록
ord-8cc00b3d628d41adb3ac80e9cafeace1
출처 데이터셋
uspto-grants-1990_05
특허 번호
US04927968

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