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Hydrogen Bromide → HCID 20267383, 화합물

HRID 1719640
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HRID 1719640 반응식
C([NH:4][C:5]1[CH:10]=[C:9]([NH:11][C:12](=[O:14])[CH3:13])[CH:8]=[CH:7][C:6]=1[O:15][CH2:16][CH2:17][CH3:18])(=O)C.NC1C=C(N)C=CC=1OCCC.C([O-])(=O)C.[Mg+2].C([O-])(=O)C.[BrH:40]>C(O)C>[BrH:40].[CH2:16]([O:15][C:6]1[C:5]([NH2:4])=[CH:10][C:9]([NH:11][C:12](=[O:14])[CH3:13])=[CH:8][CH:7]=1)[CH2:17][CH3:18]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 260Hydrogen BromideHCID 8896Magnesium AcetateHCID 1536932,4-DiaminopropoxybenzeneHCID 566908122,4-Bis-acetylamino-1-n-propoxybenzene

생성물 1

HCID 20267383HCID 20267383, 화합물수율 88.9%

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
25 °C

실험 절차

208 parts of dried crude 6-n-propoxy-3-acetylamino-aniline obtained according to Example 7 of European Pat. No. 0,011,048 (containing, in addition to 190.3 parts of target product, 8.8 parts of 2,4-bis-acetylamino-1-n-propoxybenzene and 3.5 parts of 2,4-diamino-1-n-propoxybenzene, as well as small amounts of magnesium acetate and oxidative decomposition products) are dissolved in 300 parts of ethanol at 50° C., with stirring, and, after the solution has been cooled to 25° C., 170 parts of 48% strength hydrobromic acid are added dropwise in the course of 1.5 hours. The precipitate which has separated out is filtered off with suction at 0°-5° C., washed with two portions of 60 parts of ethanol and dried in vacuo. 257.1 parts of 6-n-propoxy-3-acetylamino-aniline hydrobromide (no impurities detectable by HPLC, purity by diazotization: 99.4%) are obtained, which corresponds to a yield of 88.9% of theory (based on the crude feed product) or 97.2% of theory (based on the target product contained therein).

후처리

  1. dry with material208 parts of dried crude 6-n-propoxy-3-acetylamino-aniline
  2. customobtained
  3. customThe precipitate which has separated out
  4. filtrationis filtered off with suction at 0°-5° C.
  5. washwashed with two portions of 60 parts of ethanol
  6. customdried in vacuo

출처 및 근거

ORD 기록
ord-bdd1d955f3904ae3b66064748f09f04a
출처 데이터셋
uspto-grants-1985_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04540815

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