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

HRID 2402545

反応式

HRID 2402545 の反応式
[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

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 178503042HCID 178503042、化合物触媒HCID 1140Toluene溶媒

実験手順

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%)

後処理

  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.

出典と根拠

ORDレコード
ord-fdbf1d2967f846c0bd4e9de657feda77
出典データセット
uspto-grants-2014_08
特許番号
US08796447B2

関連ノート

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