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Water → HCID 18326572, 화합물

HRID 1250585
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HRID 1250585 반응식
[CH2:1]([NH:4][C:5]1[C:14]2[C:9](=[CH:10][CH:11]=[C:12]([N+:15]([O-:17])=[O:16])[CH:13]=2)[N:8]=[C:7](Cl)[N:6]=1)[CH:2]=[CH2:3].Cl.[CH2:20]([NH2:24])/[CH:21]=[CH:22]/[CH3:23].C(N(CC)CC)C.O>C(#N)C>[CH2:1]([NH:4][C:5]1[C:14]2[C:9](=[CH:10][CH:11]=[C:12]([N+:15]([O-:17])=[O:16])[CH:13]=2)[N:8]=[C:7]([NH:24][CH2:20]/[CH:21]=[CH:22]/[CH3:23])[N:6]=1)[CH:2]=[CH2:3]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 12602976(2E)-but-2-en-1-amine hydrochlorideHCID 183264874-Allylamino-2-chloro-6-nitroquinazoline

생성물 1

HCID 18326572HCID 18326572, 화합물수율 80.9%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

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온도
50 °C

실험 절차

150 mg (0.57 mmol) of 4-allylamino-2-chloro-6-nitroquinazoline was dissolved in 2 ml of acetonitrile, and 305 mg (2.83 mmol) of trans-2-butenylamine hydrochloride and 0.39 ml (2.83 mmol) of triethylamine were added thereto, followed by stirring at 50° C. for 6 hours. To the reaction solution was water added, followed by extraction with ethyl acetate, washing with brine and drying over anhydrous sodium sulfate. After the solvent was distilled off, the residue was purified by a silica gel column to give 138 mg (yield: 80.9%) of the title compound.

후처리

  1. additionadded
  2. extractionfollowed by extraction with ethyl acetate
  3. washwashing with brine
  4. dry with materialdrying over anhydrous sodium sulfate
  5. distillationAfter the solvent was distilled off
  6. customthe residue was purified by a silica gel column

출처 및 근거

ORD 기록
ord-2209ba33f2764431a12fe9c21fc2b7f4
출처 데이터셋
uspto-grants-2002_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06339089B2

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