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Diisopropylethylamine → (+/-)-2-[2-[[4-[5-(7-Ethyl-2-methyl-4H-benzo[5,6]cyclohept[1,2-d]oxazol-4-yl)-3,4-dihydro-2,4-dioxo-1(2H)-pyrimidinyl]pyrimidin-2-yl]amino]acetylamino]-4-thiazoleacetic acid, ethyl ester

HRID 324403
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인쇄 미리보기

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HRID 324403 반응식
Cl[C:2]1[N:7]=[C:6]([N:8]2[CH:13]=[C:12]([CH:14]3[C:20]4[N:21]=[C:22]([CH3:24])[O:23][C:19]=4[CH:18]=[CH:17][C:16]4[CH:25]=[C:26]([CH2:29][CH3:30])[CH:27]=[CH:28][C:15]3=4)[C:11](=[O:31])[NH:10][C:9]2=[O:32])[CH:5]=[CH:4][N:3]=1.C(N(CC)C(C)C)(C)C.[CH2:42]([O:44][C:45](=[O:57])[CH2:46][C:47]1[N:48]=[C:49]([NH:52][C:53](=[O:56])[CH2:54][NH2:55])[S:50][CH:51]=1)[CH3:43]>CN1CCCC1=O>[CH2:29]([C:26]1[CH:27]=[CH:28][C:15]2[CH:14]([C:12]3[C:11](=[O:31])[NH:10][C:9](=[O:32])[N:8]([C:6]4[CH:5]=[CH:4][N:3]=[C:2]([NH:55][CH2:54][C:53]([NH:52][C:49]5[S:50][CH:51]=[C:47]([CH2:46][C:45]([O:44][CH2:42][CH3:43])=[O:57])[N:48]=5)=[O:56])[N:7]=4)[CH:13]=3)[C:20]3[N:21]=[C:22]([CH3:24])[O:23][C:19]=3[CH:18]=[CH:17][C:16]=2[CH:25]=1)[CH3:30]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 81531Diisopropylethylamine2회HCID 54551034Ethyl 2-(2-(2-aminoacetamido)thiazol-4-yl)acetateHCID 88152174(+/-)-1-(2-Chloropyrimidin-4-yl)-5-(7-ethyl-2-methyl-4H-benzo[5,6]cyclohepta[1,2-d]oxazol-4-yl)-2,4(1H,3H)-pyrimidinedione

생성물 1

HCID 131722503(+/-)-2-[2-[[4-[5-(7-Ethyl-2-methyl-4H-benzo[5,6]cyclohept[1,2-d]oxazol-4-yl)-3,4-dihydro-2,4-dioxo-1(2H)-pyrimidinyl]pyrimidin-2-yl]amino]acetylamino]-4-thiazoleacetic acid, ethyl ester

시약·촉매·용매 1

HCID 13387N-methyl-2-pyrrolidone용매

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온도
90 °C

실험 절차

A mixture of the products from steps (viii) (0.65 g) and (ix) (1.025 g) and N,N-diisopropylethylamine (1.26 ml) in N-methylpyrrolidin-2-one (10 ml) was stirred at 90° C. for 24 hours. A further 0.342 g of product from step (ix) and N,N-diisopropylethylamine (0.5 ml) was added and heating continued for a further 24 hours. The solution was partitioned between 1N hydrochloric acid and ethyl acetate. The organic layer was washed with water, dried (MgSO4) and evaporated to give a brown oil which was purified by chromatography eluting with ethyl acetate.

후처리

  1. temperatureheating
  2. waitcontinued for a further 24 hours
  3. customThe solution was partitioned between 1N hydrochloric acid and ethyl acetate
  4. washThe organic layer was washed with water
  5. dry with materialdried (MgSO4)
  6. customevaporated
  7. customto give a brown oil which
  8. customwas purified by chromatography
  9. washeluting with ethyl acetate

출처 및 근거

ORD 기록
ord-0009afbe1b7e40a7879fbe983f6a5173
출처 데이터셋
uspto-grants-2001_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06218376B1

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