Hydrochloric Acid → HCID 67316013、化合物

HRID 1012992ノート

反応式

HRID 1012992 の反応式
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]

参加物

6

反応物 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

生成物 1

HCID 67316013HCID 67316013、化合物

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

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+).

後処理

  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

出典と根拠

ORDレコード
ord-f3c7804495ef432f8916c210c6bb21f3
出典データセット
uspto-grants-2011_07
特許番号
US07981879B2

反応ノート

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