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Butoxycarbonylpentyl isocyanate → HCID 19848120, 화합물

HRID 845251
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HRID 845251 반응식
[CH:1]([O:4][C:5]([C:7]1[S:8][C:9]([C:14]([O:16][CH:17]([CH3:19])[CH3:18])=[O:15])=[C:10]([OH:13])[C:11]=1[CH3:12])=[O:6])([CH3:3])[CH3:2].[CH2:20]([O:24][C:25]([CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][N:32]=[C:33]=[O:34])=[O:26])[CH2:21][CH2:22][CH3:23]>C(#N)C.C1N2CCN(CC2)C1>[CH:1]([O:4][C:5]([C:7]1[S:8][C:9]([C:14]([O:16][CH:17]([CH3:19])[CH3:18])=[O:15])=[C:10]([O:13][C:33]([NH:32][CH2:31][CH2:30][CH2:29][CH2:28][CH2:27][C:25]([O:24][CH2:20][CH2:21][CH2:22][CH3:23])=[O:26])=[O:34])[C:11]=1[CH3:12])=[O:6])([CH3:2])[CH3:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 13836475Butoxycarbonylpentyl isocyanateHCID 54703303HCID 54703303, 화합물

생성물 1

HCID 19848120HCID 19848120, 화합물수율 93.4%

시약·촉매·용매 2

HCID 9237Dabco촉매HCID 6342Acetonitrile용매2회

실험 절차

10.0 g of 2,5-bis-(isopropoxycarbonyl)-3-methyl-4-hydroxythiophene, 20 ml of anhydrous acetonitrile, 15 g of butoxycarbonylpentyl isocyanate (b.p. 149°-151°/13 millibar) and 100 mg of triethylene diamine are maintained at 100° C. for 18 hours. The mixture is diluted with 20 ml of acetonitrile. To remove the excess butoxycarbonylpentyl isocyanate, the reaction mixture is shaken three times with 50 ml of ligroin in each case. The acetonitrile phase is evaporated in vacuo. The evaporation residue is dried at 100° C./0.1 mbar. 16.3 g of 2,5-bis-(isopropoxycarbonyl)-3-methyl-4-[5-(butyloxycarbonyl)pentylaminocarbonyloxy]-thiophene are obtained as a viscous material.

후처리

  1. customTo remove the excess butoxycarbonylpentyl isocyanate
  2. customThe acetonitrile phase is evaporated in vacuo
  3. customThe evaporation residue is dried at 100° C./0.1 mbar

출처 및 근거

ORD 기록
ord-b83ad34bed224b22ae0cba75b9997c82
출처 데이터셋
uspto-grants-1988_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04757085

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