Water → 3-[(Tert-butoxycarbonyl-methyl-amino)-methyl]-benzoic acid

HRID 901947

반응식

HRID 901947 반응식
O.[OH-].[Li+].O.[CH3:5][N:6]([CH2:14][C:15]1[CH:20]=[CH:19][CH:18]=[C:17]([C:21]([O:23]C)=[O:22])[CH:16]=1)[C:7](=[O:13])[O:8][C:9]([CH3:12])([CH3:11])[CH3:10]>O1CCOCC1>[C:21]([C:17]1[CH:16]=[C:15]([CH:20]=[CH:19][CH:18]=1)[CH2:14][N:6]([CH3:5])[C:7](=[O:13])[O:8][C:9]([CH3:11])([CH3:12])[CH3:10])([OH:23])=[O:22]

참가 물질

5

반응물 3

HCID 962WaterHCID 168937Lithium hydroxide, monohydrateHCID 59700597Methyl 3-(((tert-butoxycarbonyl)(methyl)amino)methyl)benzoate

생성물 1

HCID 224502433-[(Tert-butoxycarbonyl-methyl-amino)-methyl]-benzoic acid수율 95%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

Lithium hydroxide monohydrate (420 mg, 10 mmol) and water (15 ml) were added to a solution of tert-butyl N-methyl-N-(3-(methyloxycarbonyl)benzyl)carbamate (1.6 g, 5.6 mmol) in dioxan (20 ml) and the mixture was stirred for 2 h. The dioxan was removed in vacuo and the residue was taken up in 0.3N potassium hydrogen sulphate. The mixture was extracted with ethyl acetate and the organic phase was washed with water and brine, dried and reduced to afford tert-butyl N-(3-carboxybenzyl)-N-methylcarbamate (1.4 g, 95%).

후처리

  1. customThe dioxan was removed in vacuo
  2. extractionThe mixture was extracted with ethyl acetate
  3. washthe organic phase was washed with water and brine
  4. customdried

출처 및 근거

ORD 기록
ord-bfed7b5070074d4db80fec8494a809e6
출처 데이터셋
uspto-grants-2008_04
특허 번호
US07365065B2

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