홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Hydrochloric Acid → Tert-butyl 7-(3,4-dichlorophenyl)-7-(hydroxymethyl)-6-oxo-1,4-oxazepane-4-carboxylate

HRID 1022828
노트
인쇄 미리보기

반응식

HRID 1022828 반응식
[OH-:1].[K+].[Cl:3][C:4]1[CH:5]=[C:6]([CH:11]2[O:17][CH2:16][CH2:15][N:14]([C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19])[CH2:13][C:12]2=[O:25])[CH:7]=[CH:8][C:9]=1[Cl:10].[CH2:26]=O.Cl>C(O)C.CS(C)=O.[Cl-].[Na+].O>[Cl:3][C:4]1[CH:5]=[C:6]([C:11]2([CH2:26][OH:1])[O:17][CH2:16][CH2:15][N:14]([C:18]([O:20][C:21]([CH3:22])([CH3:24])[CH3:23])=[O:19])[CH2:13][C:12]2=[O:25])[CH:7]=[CH:8][C:9]=1[Cl:10]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 313Hydrochloric AcidHCID 712FormaldehydeHCID 14797Potassium HydroxideHCID 66976649HCID 66976649, 화합물

생성물 1

HCID 66976886Tert-butyl 7-(3,4-dichlorophenyl)-7-(hydroxymethyl)-6-oxo-1,4-oxazepane-4-carboxylate수율 456.5%

시약·촉매·용매 3

HCID 679
Dimethyl Sulfoxide
용매
HCID 702Ethanol용매
HCID 57417360Sodium chloride; water용매

실험 절차

Potassium hydroxide (40 mg) was dissolved in ethanol (1.25 ml), and the solution was diluted with DMSO (25 mL). To this solution were added tert-butyl 7-(3,4-dichlorophenyl)-6-oxo-1,4-oxazepane-4-carboxylate (2.60 g) and paraformaldehyde (267 mg), and the mixture was stirred at room temperature for 30 min. The reaction solution was neutralized with 1 N hydrochloric acid, brine was added, and the mixture was extracted with ethyl acetate. The organic layer was washed twice with brine, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel chromatography (hexane/ethyl acetate) to give the title compound (1.27 g).

후처리

  1. additionwas added
  2. extractionthe mixture was extracted with ethyl acetate
  3. washThe organic layer was washed twice with brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customthe solvent was evaporated under reduced pressure
  6. customThe residue was purified by silica gel chromatography (hexane/ethyl acetate)

출처 및 근거

ORD 기록
ord-2a60eb57a36b403b8f0a817f4aac6a6e
출처 데이터셋
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08722662B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트