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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Dimethyl Sulfoxide → HCID 22241385, 화합물

HRID 892219
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HRID 892219 반응식
C(Cl)(=O)C(Cl)=O.CS(C)=O.[OH:11][CH2:12][C:13]1[C:40]([CH3:41])=[CH:39][CH:38]=[CH:37][C:14]=1[CH2:15][O:16][C:17]1[CH:18]=[C:19]([CH:34]=[CH:35][CH:36]=1)[O:20][CH2:21][C:22]1[N:31]([CH3:32])[C:30](=[O:33])[C:29]2[C:24](=[CH:25][CH:26]=[CH:27][CH:28]=2)[N:23]=1.C(N(CC)CC)C>ClCCl>[CH3:41][C:40]1[CH:39]=[CH:38][CH:37]=[C:14]([CH2:15][O:16][C:17]2[CH:36]=[CH:35][CH:34]=[C:19]([O:20][CH2:21][C:22]3[N:31]([CH3:32])[C:30](=[O:33])[C:29]4[C:24](=[CH:25][CH:26]=[CH:27][CH:28]=4)[N:23]=3)[CH:18]=2)[C:13]=1[CH:12]=[O:11]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 679Dimethyl SulfoxideHCID 8471TriethylamineHCID 65578Oxalyl chlorideHCID 22241343HCID 22241343, 화합물

생성물 1

HCID 22241385HCID 22241385, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a cooled (−78° C.) solution of oxalyl chloride (2.5 mL, 1.75 M in CH2Cl2) is added, dropwise, DMSO (80 mL). On complete addition, a solution of 2-[3-(2-hydroxymethyl-3-methyl-1 benzyloxy)-phenoxymethyl]-3-methyl-3H-quinazolin-4-one (120 mg, 0.28 mmol, example 101) in dichloromethane (1 mL) is added dropwise. This solution is stirred for 5 min then triethylamine (276 mL, 2 mmol) is added in one portion. The cold bath is removed and stirring continued for 10 min. The mixture is then diluted with ethyl acetate, washed with water and brine, dried over MgSO4 and concentrated to give the title compound as a solid. MS (ESI) 415 (M+H)+.

후처리

  1. additionis added
  2. additionOn complete addition
  3. customThe cold bath is removed
  4. stirringstirring
  5. waitcontinued for 10 min
  6. additionThe mixture is then diluted with ethyl acetate
  7. washwashed with water and brine
  8. dry with materialdried over MgSO4
  9. concentrationconcentrated

출처 및 근거

ORD 기록
ord-13be80ba75b14c159c8ef917847a14be
출처 데이터셋
uspto-grants-2006_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07005440B1

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