Triethylamine → HCID 178512291, 화합물

HRID 1157368노트

반응식

HRID 1157368 반응식
[NH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][O:8][C:9]1[CH:10]=[N:11][CH:12]=[CH:13][CH:14]=1.CS[C:17](=[N:21][C:22]1[CH:27]=[CH:26][N:25]=[CH:24][CH:23]=1)[NH:18][C:19]#[N:20].C(N(CC)CC)C>CN(C1C=CN=CC=1)C.N1C=CC=CC=1>[N:11]1[CH:12]=[CH:13][CH:14]=[C:9]([O:8][CH2:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2][NH:1][C:17]([NH:18][C:19]#[N:20])=[N:21][C:22]2[CH:27]=[CH:26][N:25]=[CH:24][CH:23]=2)[CH:10]=1

참가 물질

6

반응물 3

HCID 8471TriethylamineHCID 155219651-Cyano-2-methyl-3-pyridin-4-yl-isothioureaHCID 231324436-(Pyridin-3-yloxy)-hexylamine

생성물 1

HCID 178512291HCID 178512291, 화합물

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 1049Pyridine용매2회

반응 조건

온도
60 °C

실험 절차

A mixture of 3-[6-amino-1-hexyl-oxy]-pyridine (150 mg), S-methyl-N-cyano-N′-4-pyridyl-isothiourea (123 mg), triethylamine (0.18 ml), 4-(N,N-dimethylamino)-pyridine (3.5 mg) and pyridine (5 ml) was stirred overnight at 60° C. After cooling to room temperature the pyridine was removed by evaporation twice with toluene in vacuo and the residue was distributed between water and ethyl acetate. The organic phase was dried and evaporated to yield a crude product which was purified by chromatography on silica gel with ethyl acetate/methanol/aqueous ammonia (40:10:2.5) as eluent. The pure fractions were pooled and evaporated to give the title compound which crystallised from ethyl acetate.

후처리

  1. customwas removed by evaporation twice with toluene in vacuo
  2. customThe organic phase was dried
  3. customevaporated
  4. customto yield a crude product which
  5. customwas purified by chromatography on silica gel with ethyl acetate/methanol/aqueous ammonia (40:10:2.5) as eluent
  6. customevaporated

출처 및 근거

ORD 기록
ord-806d10be473144599b5d5751c7d4febb
출처 데이터셋
uspto-grants-2010_10
특허 번호
US07807682B2

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