Triethylamine → HCID 178512288, 화합물

HRID 555329노트

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HRID 555329 반응식
[NH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][N:8]1[C:17]2[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=2)[CH:11]=[CH:10][C:9]1=[O:18].CS[C:21](=[N:25][C:26]1[CH:31]=[CH:30][N:29]=[CH:28][CH:27]=1)[NH:22][C:23]#[N:24].C(N(CC)CC)C>CN(C1C=CN=CC=1)C.N1C=CC=CC=1>[O:18]=[C:9]1[CH:10]=[CH:11][C:12]2[C:17](=[CH:16][CH:15]=[CH:14][CH:13]=2)[N:8]1[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2][NH:1][C:21]([NH:22][C:23]#[N:24])=[N:25][C:26]1[CH:31]=[CH:30][N:29]=[CH:28][CH:27]=1

참가 물질

6

반응물 3

HCID 8471TriethylamineHCID 155219651-Cyano-2-methyl-3-pyridin-4-yl-isothioureaHCID 45117461HCID 45117461, 화합물

생성물 1

HCID 178512288HCID 178512288, 화합물

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 1049Pyridine용매2회

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온도
60 °C

실험 절차

A mixture of 1-(6-amino-1-hexyl)-1,2-dihydroquinoline-2-one (320 mg), S-methyl-N-cyano-N′-4-pyridyl-isothiourea (210 mg), triethylamine (0.31 ml), 4-(N,N-dimethylamino)-pyridine (7 mg) and pyridine (10 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 (40:10:1.25) as eluent. The pure fractions were pooled, evaporated, triturated with ethyl acetate and dried in vacuo to give the title compound.

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 (40:10:1.25) as eluent
  6. customevaporated
  7. customtriturated with ethyl acetate
  8. customdried in vacuo

출처 및 근거

ORD 기록
ord-9208e559f07e4b7e954d9343a3ffba9f
출처 데이터셋
uspto-grants-2011_11
특허 번호
US08053446B2

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