Hydrochloric Acid → HCID 67316013, 화합물

HRID 1012992노트

반응식

HRID 1012992 반응식
C([N:8]([CH3:33])[CH:9]1[CH2:15][N:14]([C:16]([O:18][C:19]([CH3:22])([CH3:21])[CH3:20])=[O:17])[CH2:13][CH2:12][N:11]2[C:23](=[O:32])[C:24]([OH:31])=[C:25]([C:27](OC)=[O:28])[N:26]=[C:10]12)C1C=CC=CC=1.Cl.[Cl:35][C:36]1[CH:37]=[C:38]([CH:41]=[CH:42][C:43]=1[CH3:44])[CH2:39][NH2:40]>CO.[Pd]>[Cl:35][C:36]1[CH:37]=[C:38]([CH:41]=[CH:42][C:43]=1[CH3:44])[CH2:39][NH:40][C:27]([C:25]1[N:26]=[C:10]2[CH:9]([NH:8][CH3:33])[CH2:15][N:14]([C:16]([O:18][C:19]([CH3:21])([CH3:20])[CH3:22])=[O:17])[CH2:13][CH2:12][N:11]2[C:23](=[O:32])[C:24]=1[OH:31])=[O:28]

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 106225Benzenemethanamine, 3-chloro-4-methyl-HCID 673173728-tert-butyl 2-methyl 10-[benzyl(methyl)amino]-3-hydroxy-4-oxo-6,7,9,10-tetrahydropyrimido[1,2-d][1,4]diazepine-2,8(4H)-dicarboxylate

생성물 1

HCID 67316013HCID 67316013, 화합물

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

8-tert-butyl 2-methyl 10-[benzyl(methyl)amino]-3-hydroxy-4-oxo-6,7,9,10-tetrahydropyrimido[1,2-d][1,4]diazepine-2,8(4H)-dicarboxylate (see Example 11, Steps 1-4) was dissolved in MeOH, treated with 1 N HCl (1 eq.) and stirred overnight under an H2 atmosphere in the presence of 10% Pd/C. The catalyst was then filtered off through celite, and the filtrate was concentrated under reduced pressure. MS (ES) C16H24N4O6 requires 368. Found: 369 (M+H+). The crude organic product was taken in methanol and treated with 1.2 eq. of 3-chloro-4-methyl-benzylamine and resulting mixture was refluxed overnight. After cooling to room temperature, evaporation of volatiles under reduced pressure yielded title product which was directly taken in the next step. MS (ES) C23H30ClN5O5 requires 491. Found: 492 (M+H+).

후처리

  1. filtrationThe catalyst was then filtered off through celite
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. customresulting mixture
  4. temperaturewas refluxed overnight
  5. customevaporation of volatiles under reduced pressure

출처 및 근거

ORD 기록
ord-f3c7804495ef432f8916c210c6bb21f3
출처 데이터셋
uspto-grants-2011_07
특허 번호
US07981879B2

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