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

Methanol → HCID 22631041, 화합물

HRID 2416455
노트
인쇄 미리보기

반응식

HRID 2416455 반응식
CC(C[AlH]CC(C)C)C.[N:10]1([C:15]2[N:20]=[CH:19][C:18](/[CH:21]=[CH:22]/[CH:23]=[O:24])=[CH:17][CH:16]=2)[CH:14]=[CH:13][CH:12]=[N:11]1.CO.C(C(C(C([O-])=O)O)O)([O-])=O.[Na+].[K+]>C1(C)C=CC=CC=1.ClCCl.C(OCC)(=O)C>[N:10]1([C:15]2[N:20]=[CH:19][C:18](/[CH:21]=[CH:22]/[CH2:23][OH:24])=[CH:17][CH:16]=2)[CH:14]=[CH:13][CH:12]=[N:11]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 887MethanolHCID 14487Diisobutylaluminum hydrideHCID 9855836Potassium sodium tartarateHCID 22630936HCID 22630936, 화합물

생성물 1

HCID 22631041HCID 22631041, 화합물수율 60.1%

시약·촉매·용매 3

HCID 1140Toluene용매
HCID 6344
Dichloromethane
용매
HCID 8857Ethyl Acetate용매

실험 절차

DIBAL (1.0 M solution in toluene, 3.10 mL, 3.10 mmol) was added dropwise to a suspension of the compound from step B (350 mg, 1.53 mmol) in toluene (10 mL) and dichloromethane (4 mL) at −78° C. and the mixture was stirred for 2 h at that temperature. Methanol (1 mL) was added and the mixture was poured into a stirring mixture of ethyl acetate (20 mL) and 10% aq. potassium sodium tartrate (20 mL) and stirred for 1 h at RT. The organic layer was washed with brine (20 mL), dried (Na2SO4), and concentrated. Purification by chromatography (SiO2, 1:1 hexane/ethyl acetate) yielded 185 mg (59%) of the title compound. MS 202 (M+H)+.

후처리

  1. stirringstirred for 1 h at RT
  2. washThe organic layer was washed with brine (20 mL)
  3. dry with materialdried (Na2SO4)
  4. concentrationconcentrated
  5. customPurification by chromatography (SiO2, 1:1 hexane/ethyl acetate)

출처 및 근거

ORD 기록
ord-d0884dbc6407468d823c493ed474bf1c
출처 데이터셋
uspto-grants-2004_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06825170B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트