Phosphoric Acid → m-Aminobenzylamine phosphoric acid salt

HRID 580086노트

반응식

HRID 580086 반응식
[N+:1]([C:4]1[CH:5]=[C:6]([CH:10]=[CH:11][CH:12]=1)[CH:7]=[N:8]O)([O-])=O.[P:13](=[O:17])([OH:16])([OH:15])[OH:14].[H][H]>[Pt].C(O)C(C)C>[P:13](=[O:14])([OH:17])([OH:16])[OH:15].[NH2:1][C:4]1[CH:5]=[C:6]([CH:10]=[CH:11][CH:12]=1)[CH2:7][NH2:8]

참가 물질

6

반응물 3

HCID 1004Phosphoric AcidHCID 2191323-NitrobenzaldoximeHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 20136024m-Aminobenzylamine phosphoric acid salt수율 86.1%

시약·촉매·용매 2

HCID 23939Platinum촉매HCID 6560Isobutanol용매

실험 절차

33.2 g (0.2 mol) of this m-nitrobenzaldoxime, 70 g (0.35 mol) of a 50% aqueous solution of phosphoric acid, 0.3 g of a 10% Pt-C catalyst and 300 ml of isobutanol were charged into a hermetically sealed glass container and vigorously stirred while charging hydrogen. Reaction was continued at temperatures of 25° to 30° C. for 18 hours and 23 l of hydrogen was absorbed. The reaction mixture from which crystals deposited was filtered and 54.8 g of crude m-aminobenzylamine phosphoric acid salt (yield 86.1%) was obtained. This crude m-aminobenzylamine phosphoric acid salt was recrystallized from a 50% methanol-water solution and pure m-aminobenzylamine phosphoric acid salt of white and flaky crystals was obtained. M.P. 210°-213° C.

후처리

  1. customReaction
  2. custom23 l of hydrogen was absorbed
  3. filtrationThe reaction mixture from which crystals deposited was filtered

출처 및 근거

ORD 기록
ord-08575de4e6da4cee95441ab564e25e18
출처 데이터셋
uspto-grants-1988_06
특허 번호
US04751328

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