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Hydrochloric Acid → 5-Methyl-2,5,7-triazaspiro[3.4]octan-8-one

HRID 915846
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HRID 915846 반응식
C([N:14]1[CH2:17][C:16]2([C:21](=[O:22])[N:20]=[CH:19][N:18]2[CH3:23])[CH2:15]1)(C1C=CC=CC=1)C1C=CC=CC=1.[ClH:24]>CO.C(OCC)C.[OH-].[OH-].[Pd+2]>[ClH:24].[CH3:23][N:18]1[CH2:19][NH:20][C:21](=[O:22])[C:16]21[CH2:17][NH:14][CH2:15]2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 2

HCID 313Hydrochloric AcidHCID 21905771HCID 21905771, 화합물

생성물 1

HCID 1317260095-Methyl-2,5,7-triazaspiro[3.4]octan-8-one

시약·촉매·용매 3

HCID 9942167Palladium hydroxide촉매HCID 887Methanol용매HCID 3283Diethyl Ether용매2회

실험 절차

To a solution of 2-benzhydryl-5-methyl-2,5,7-triazaspiro[3.4]oct-6-en-8-one (I-2A-69c; 189 mg, 0.619 mmol) in methanol (30 ml) was added 1 M HCl in diethyl ether (1.3 ml). After the addition of 20% Pd(OH)2 on carbon (50% water; 95 mg), the mixture was placed on a Parr® shaker and then reduced (50 psi H2) at room temperature for 5 hours. The reaction mixture was filtered through a 0.45 PM disk, and then concentrated, in vacuo, to give a solid. Trituration from diethyl ether afforded I-2A-69d (124 mg, 94%) as an off-white solid: +APcl MS (M+1) 142.0; 1H NMR (400 MHz, CD3OD) δ 4.38 (d, J=12.0 Hz, 2H), 4.17 (s, 2H), 4.13 (d, J=12.5 Hz, 2H), 2.71 (s, 3H).

후처리

  1. customat room temperature
  2. customfor 5 hours
  3. filtrationThe reaction mixture was filtered through a 0.45 PM disk
  4. concentrationconcentrated, in vacuo
  5. customto give a solid

출처 및 근거

ORD 기록
ord-d86ad0b1d42248f281bd39a505b6b983
출처 데이터셋
uspto-grants-2007_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07268133B2

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