2-Methyl-2-butene → 1-Ethyl-3,3,5-trimethyl-2,4-dioxo-2,3,4,5-tetrahydro-1H-benzo[b][1,4]diazepine-7-carboxylic acid

HRID 1504123노트

반응식

HRID 1504123 반응식
[CH2:1]([N:3]1[C:9](=[O:10])[C:8]([CH3:12])([CH3:11])[C:7](=[O:13])[N:6]([CH3:14])[C:5]2[CH:15]=[C:16]([CH:19]=[O:20])[CH:17]=[CH:18][C:4]1=2)[CH3:2].CC(=CC)C.P([O-])(O)(O)=[O:27].[Na+].Cl([O-])=O.[Na+]>O.C(O)(C)(C)C>[CH2:1]([N:3]1[C:9](=[O:10])[C:8]([CH3:12])([CH3:11])[C:7](=[O:13])[N:6]([CH3:14])[C:5]2[CH:15]=[C:16]([C:19]([OH:27])=[O:20])[CH:17]=[CH:18][C:4]1=2)[CH3:2]

참가 물질

7

반응물 4

HCID 105532-Methyl-2-buteneHCID 23668197Sodium ChloriteHCID 23672064Monosodium phosphateHCID 866704761-ethyl-3,3,5-trimethyl-2,4-dioxo-2,3,4,5-tetrahydro-1H-benzo[b][1,4]diazepine-7-carbaldehyde

생성물 1

HCID 669604471-Ethyl-3,3,5-trimethyl-2,4-dioxo-2,3,4,5-tetrahydro-1H-benzo[b][1,4]diazepine-7-carboxylic acid수율 44%

시약·촉매·용매 2

HCID 962Water용매2회HCID 6386tert-Butanol용매

실험 절차

To a t-butanol (20 ml) and H2O (5 ml) solution of 1-ethyl-3,3,5-trimethyl-2,4-dioxo-2,3,4,5-tetrahydro-1H-benzo[b][1,4]diazepine-7-carbaldehyde (2.25 g) and 2-methyl-2-butene(3.25 ml) were added sodium dihydrogenphosphate (0.92 g) and sodium chlorite (2.081 g), and the mixture was stirred at room temperature overnight. Water was added to the reaction mixture, followed by extraction using ethyl acetate. The organic layer was dried with sodium sulfate, and was condensed under reduced pressure to give the title compound (0.98 g) as a white powder.

후처리

  1. extractionfollowed by extraction
  2. dry with materialThe organic layer was dried with sodium sulfate
  3. customcondensed under reduced pressure

출처 및 근거

ORD 기록
ord-31d7eadebcc448749cfa89e3608edf4c
출처 데이터셋
uspto-grants-2015_12
특허 번호
US09212187B2

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