Hydrochloric Acid → 5-benzyloxy-N1-methylbenzene-1,2-diamine hydrochloride

HRID 2402545

반응식

HRID 2402545 반응식
[CH2:1]([O:8][C:9]1[CH:10]=[CH:11][C:12]([N+:17]([O-])=O)=[C:13]([CH:16]=1)[NH:14][CH3:15])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[ClH:20]>[C].[Pt].C1(C)C=CC=CC=1>[ClH:20].[CH2:1]([O:8][C:9]1[CH:16]=[C:13]([NH:14][CH3:15])[C:12]([NH2:17])=[CH:11][CH:10]=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 679540515-benzyloxy-N-methyl-2-nitroaniline

생성물 1

HCID 679539765-benzyloxy-N1-methylbenzene-1,2-diamine hydrochloride수율 91%

시약·촉매·용매 2

HCID 178503042HCID 178503042, 화합물촉매HCID 1140Toluene용매

실험 절차

5% platinum carbon (2.15 g, water content: 53.1%) was added to a toluene (300 mL) suspension of 5-benzyloxy-N-methyl-2-nitroaniline (20 g, 77.4 mmol), and catalytic hydrogenation reaction was performed at 4 atm. The reaction solution was filtered to remove a catalyst. The catalyst was washed with 2-propanol (40 mL), and the washing liquid was added to the precedent filtrate. Under ice cooling, concentrated hydrochloric acid (6.6 mL, 77.4 mmol) was added to the mixture, and the mixture was stirred under the same temperature for 30 minutes. The resulting precipitated crystals were collected by filtration, then washed with 2-propanol (60 mL), and dried at 50° C., thereby obtaining 18.6 g of a light-pink, crystal target compound (yield: 91%)

후처리

  1. filtrationThe reaction solution was filtered
  2. customto remove a catalyst
  3. washThe catalyst was washed with 2-propanol (40 mL)
  4. additionthe washing liquid was added to the precedent filtrate
  5. customThe resulting precipitated crystals
  6. filtrationwere collected by filtration
  7. washwashed with 2-propanol (60 mL)
  8. customdried at 50° C.

출처 및 근거

ORD 기록
ord-fdbf1d2967f846c0bd4e9de657feda77
출처 데이터셋
uspto-grants-2014_08
특허 번호
US08796447B2

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