Ethanol → HCID 178496020, 화합물

HRID 909910노트

반응식

HRID 909910 반응식
[C:1]([C:3]1[CH:4]=[C:5]([CH:26]=[CH:27][CH:28]=1)[CH2:6][CH2:7][O:8][CH2:9][CH2:10][C:11]([N:13]([CH:20]1[CH2:25][CH2:24][CH2:23][CH2:22][CH2:21]1)[CH2:14][CH:15]([O:18][CH3:19])[O:16][CH3:17])=[O:12])#[N:2].C(=O)([O-])[O-].[K+].[K+].Cl.[NH2:36][OH:37].C(O)C>O>[CH:20]1([N:13]([CH2:14][CH:15]([O:18][CH3:19])[O:16][CH3:17])[C:11](=[O:12])[CH2:10][CH2:9][O:8][CH2:7][CH2:6][C:5]2[CH:26]=[CH:27][CH:28]=[C:3]([C:1](=[NH:2])[NH:36][OH:37])[CH:4]=2)[CH2:25][CH2:24][CH2:23][CH2:22][CH2:21]1

참가 물질

6

반응물 4

HCID 702EthanolHCID 11430Potassium CarbonateHCID 443297Hydroxyamine hydrochlorideHCID 581685553-(3-Cyanophenethoxy)-N-cyclohexyl-N-(2,2-dimethoxyethyl)propanamide

생성물 1

HCID 178496020HCID 178496020, 화합물

시약·촉매·용매 1

HCID 962Water용매2회

반응 조건

온도
90 °C

실험 절차

To 3-(3-cyanophenethoxy)-N-cyclohexyl-N-(2,2-dimethoxyethyl)propanamide [Example 10, Step i)] (1.5 g) within a 35 mL microwave vial was added potassium carbonate (0.80 g), hydroxylamine hydrochloride (0.402 g), water (2.5 mL) and ethanol (10 mL). The vial was sealed and stirred for 3 days before being heated at 90° C. for a total of 3 h. The reaction was diluted with water, extracted twice with ethyl acetate, which was pooled and washed twice with water, twice with brine, dried over sodium sulphate, filtered and the solvent removed to afford a colourless gum (1.7 g). This material was used in the next step directly.

후처리

  1. customThe vial was sealed
  2. extractionextracted twice with ethyl acetate, which
  3. washwashed twice with water, twice with brine
  4. dry with materialdried over sodium sulphate
  5. filtrationfiltered
  6. customthe solvent removed

출처 및 근거

ORD 기록
ord-29daa0823a604a05b6700d27bb8df2ec
출처 데이터셋
uspto-grants-2011_09
특허 번호
US08017602B2

반응 노트

불러오는 중…