2-Ethyl-1-butanol → HCID 86688760, 화합물

HRID 575932

반응식

HRID 575932 반응식
[CH2:1]([O:3][C:4](=[O:21])[CH2:5][C:6]1[CH:7]=[N:8][N:9]([CH2:12][C:13]2[CH:18]=[C:17]([Br:19])[CH:16]=[CH:15][C:14]=2[OH:20])[C:10]=1[CH3:11])[CH3:2].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.CC(OC(/N=N/C(OC(C)(C)C)=O)=O)(C)C.[CH2:57]([CH:59]([CH2:62][CH3:63])[CH2:60]O)[CH3:58]>C1COCC1.C1(C)C=CC=CC=1>[CH2:1]([O:3][C:4](=[O:21])[CH2:5][C:6]1[CH:7]=[N:8][N:9]([CH2:12][C:13]2[CH:18]=[C:17]([Br:19])[CH:16]=[CH:15][C:14]=2[O:20][CH2:60][CH:59]([CH2:62][CH3:63])[CH2:57][CH3:58])[C:10]=1[CH3:11])[CH3:2]

참가 물질

7

반응물 4

HCID 73582-Ethyl-1-butanolHCID 11776TriphenylphosphineHCID 6034084Di-tert-butyl diazene-1,2-dicarboxylateHCID 86688759HCID 86688759, 화합물

생성물 1

HCID 86688760HCID 86688760, 화합물

시약·촉매·용매 2

HCID 1140Toluene용매HCID 8028Tetrahydrofuran용매

실험 절차

A solution of [1-(5-Bromo-2-hydroxy-benzyl)-5-methyl-1H-pyrazol-4-yl]-acetic acid ethyl ester, 2, (0.18 g g 0.51 mmol), triphenylphosphine (0.26 g, 1.02 mmol), di-tert-butylazodicarboxylate (0.23 g, 1.02 mmol) and 2-ethylbutan-1-ol (0.116 ml, 1.02 mmol) in a mixture of THF (1 mL) and toluene (2 ml) was at 120° C. on microwave for 20 min. The volatiles were removed in vacuo. The crude product was purified on silica to yield {1-[5-bromo-2-(2-ethyl-butoxy)-benzyl]-5-methyl-1H-pyrazol-4-yl}-acetic acid ethyl ester, 3.

후처리

  1. customThe volatiles were removed in vacuo
  2. customThe crude product was purified on silica

출처 및 근거

ORD 기록
ord-69ba2380c54f46a6a53d84b16db946d8
출처 데이터셋
uspto-grants-2015_05
특허 번호
US09035071B2

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