Hydrochloric Acid → HCID 178448922, 화합물

HRID 1030062노트

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HRID 1030062 반응식
[CH3:1][C:2]1[N:7]=[C:6]([N:8]([CH2:46][CH2:47][CH2:48][CH3:49])[CH2:9][C:10]2[CH:15]=[CH:14][C:13]([C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=3[C:22]3[N:26](C(C4C=CC=CC=4)(C4C=CC=CC=4)C4C=CC=CC=4)[N:25]=[N:24][N:23]=3)=[CH:12][CH:11]=2)[C:5]([C:50]([O:52][CH2:53][CH3:54])=[O:51])=[CH:4][N:3]=1.Cl>C(O)C.C(Cl)(Cl)Cl>[CH3:1][C:2]1[N:7]=[C:6]([N:8]([CH2:46][CH2:47][CH2:48][CH3:49])[CH2:9][C:10]2[CH:15]=[CH:14][C:13]([C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=3[C:22]3[NH:26][N:25]=[N:24][N:23]=3)=[CH:12][CH:11]=2)[C:5]([C:50]([O:52][CH2:53][CH3:54])=[O:51])=[CH:4][N:3]=1

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 19791910Ethyl 2-methyl-4-{N-butyl-N-[{2'-(N-triphenylmethyltetrazol-5-yl)biphenyl-4-yl}methyl]amino}pyrimidine-5-carboxylate

생성물 1

HCID 178448922HCID 178448922, 화합물수율 89.8%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 6212Chloroform용매

실험 절차

The product of example 1B (3.5 g, 4.91 mmoles) was suspended in 50 ml of ethanol. Concentrated hydrochloric acid (2.1 ml) was added and the mixture was stirred for 11/2 hours at room temperature. The solution was concentrated under vacuum and the resulting residue was diluted with water. Potassium acetate was added in portions until the pH was neutral. Ether (5 ml) was added and the mixture was stirred. The sticky solid which formed was dissolved in chloroform. The chloroform solution was dried over sodium sulfate and then concentrated. The resulting residue was crystallized from ether to provide 2.08 g of the desired product. M.p. 164°-166° C. 1H NMR (CDCl3) δ0.85 (t, 3H, J=7 Hz), 1.25 (m, 2H), 1.32 (t, 3H, J=7 Hz), 1.50 (m, 2H), 2.24 (s, 3H), 3.38 (t, 2H, J=7 Hz), 4.30 (q, 2H, J=7 Hz), 4.73 (s, 2H), 7.00 (m, 4H), 7.42 (dd, 1H, J=8 Hz, J=1Hz), 7.50-7.62 (m, 2H), 7.75 (dd, 1H, J=8 Hz, J= 1Hz), 8.02 (s, 1H).

후처리

  1. concentrationThe solution was concentrated under vacuum
  2. additionthe resulting residue was diluted with water
  3. additionPotassium acetate was added in portions until the pH
  4. additionEther (5 ml) was added
  5. stirringthe mixture was stirred
  6. customThe sticky solid which formed
  7. dry with materialThe chloroform solution was dried over sodium sulfate
  8. concentrationconcentrated
  9. customThe resulting residue was crystallized from ether

출처 및 근거

ORD 기록
ord-48b4a44f8f4d4d3d96ee98db5477797d
출처 데이터셋
uspto-grants-1992_04
특허 번호
US05104877

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