1-Butanol → HCID 13715336, 화합물

HRID 1607123노트

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HRID 1607123 반응식
[C:1]([C:3]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][C:10]=2[O:12][CH2:13][CH:14]2[O:16][CH2:15]2)[NH:5][CH:4]=1)#[N:2].C(O)CCC.[O:22]([CH:26]([CH3:34])[CH2:27][C:28]([NH:30][CH2:31][CH2:32][NH2:33])=[O:29])[N+:23]([O-:25])=[O:24].[C:35]([OH:42])(=[O:41])/[CH:36]=[CH:37]/[C:38]([OH:40])=[O:39]>CO>[C:35]([OH:42])(=[O:41])/[CH:36]=[CH:37]/[C:38]([OH:40])=[O:39].[C:1]([C:3]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][C:10]=2[O:12][CH2:13][CH:14]([OH:16])[CH2:15][NH:33][CH2:32][CH2:31][NH:30][C:28](=[O:29])[CH2:27][CH:26]([O:22][N+:23]([O-:25])=[O:24])[CH3:34])[NH:5][CH:4]=1)#[N:2]

참가 물질

6

반응물 4

HCID 2631-ButanolHCID 444972Fumaric AcidHCID 12798005HCID 12798005, 화합물HCID 137153344-[(2-Aminoethyl)amino]-4-oxobutan-2-yl nitrate

생성물 1

HCID 13715336HCID 13715336, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

4.2 g. 1-(3-cyanoindol-4-yloxy)-2,3-epoxypropane (see European patent specification No. 0,045,910) are suspended in 100 ml. n-butanol, mixed with 11.5 g. 2-(3-nitroxybutanoylamino)-ethylamine and stirred for 2 days at ambient temperature. After removal of the solvent, the residue is chromatographed on silica gel with methylene chloride/methanol (95:5 v/v) and methylene chloride/methanolic ammonia solution (95:5 v/v). From the appropriate fractions, after removal of the solvent, there are obtained 4.6 g. of base. By dissolving in methanol and adding the calculated amount of fumaric acid, there are obtained, after suction filtration, 3.9 g. (40% of theory) of the desired fumarate; m.p. 155°-156° C.

후처리

  1. customAfter removal of the solvent
  2. customthe residue is chromatographed on silica gel with methylene chloride/methanol (95:5 v/v) and methylene chloride/methanolic ammonia solution (95:5 v/v)
  3. customFrom the appropriate fractions, after removal of the solvent, there
  4. customare obtained 4.6 g
  5. customare obtained
  6. filtrationafter suction filtration, 3.9 g

출처 및 근거

ORD 기록
ord-a959de38b0a8486eaf8ef1a28814a2d3
출처 데이터셋
uspto-grants-1989_09
특허 번호
US04863949

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