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Water → HCID 178494723, 화합물

HRID 1786172
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반응식

HRID 1786172 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([NH2:8])=[C:4]([C:9]2[NH:10][N:11]=[C:12]([CH2:14][O:15][CH3:16])[N:13]=2)[CH:3]=1.[Cl:17][CH2:18][C:19](Cl)=[O:20].O>C(O)(=O)C>[Cl:17][CH2:18][C:19]([NH:8][C:5]1[CH:6]=[CH:7][C:2]([Cl:1])=[CH:3][C:4]=1[C:9]1[NH:10][N:11]=[C:12]([CH2:14][O:15][CH3:16])[N:13]=1)=[O:20]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 6577Chloroacetyl chlorideHCID 178494724HCID 178494724, 화합물

생성물 1

HCID 178494723HCID 178494723, 화합물수율 87.9%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

4-Chloro-2-(5-methoxymethyl-2H-[1,2,4]triazol-3-yl)-phenylamine (60.6 g, 239 mmol) was dissolved in acetic acid (1.2 L) and chloroacetic chloride (40.4 mL, 508 mmol) was added dropwise at 14-16° C. over a period of 30 min. The resulting reaction mixture was stirred for 22 h at ambient temperature. After addition of water (600 mL) and stirring for another 90 min, the solid was filtered off and washed with water (600 mL). Drying in vacuo afforded the title compound (66.2 g, 83%) which was obtained as a yellow solid. MS: m/e=314.9 [M+H]+.

후처리

  1. customThe resulting reaction mixture
  2. stirringstirring for another 90 min
  3. filtrationthe solid was filtered off
  4. washwashed with water (600 mL)
  5. customDrying in vacuo

출처 및 근거

ORD 기록
ord-0ca5778a5a764a9084eaaad0dc9355fc
출처 데이터셋
uspto-grants-2009_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07507729B2

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