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Calcium Carbonate → 5-(Ethoxycarbonylamino)-2-(benzyloxycarbonylamino)phenol

HRID 1885495
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HRID 1885495 반응식
Cl[C:2]([O:4][CH2:5][CH3:6])=[O:3].[NH2:7][C:8]1[CH:9]=[CH:10][C:11]([NH:15][C:16]([O:18][CH2:19][C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)=[O:17])=[C:12]([OH:14])[CH:13]=1.C(=O)([O-])[O-].[Ca+2]>O1CCOCC1>[CH2:5]([O:4][C:2]([NH:7][C:8]1[CH:9]=[CH:10][C:11]([NH:15][C:16]([O:18][CH2:19][C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)=[O:17])=[C:12]([OH:14])[CH:13]=1)=[O:3])[CH3:6]
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참가 물질

5

반응물 3

HCID 10112Calcium CarbonateHCID 10928Ethyl chloroformateHCID 147457335-Amino-2-(benzyloxycarbonylamino)phenol

생성물 1

HCID 147457375-(Ethoxycarbonylamino)-2-(benzyloxycarbonylamino)phenol

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

0.14 mole (15.7 g) of ethyl chloroformate is slowly added dropwise to 0.13 mole (33 g) of 5-amino -2-(benzyloxycarbonylamino)phenol (prepared in Example 1, 2nd stage) and 7.1 g of calcium carbonate in 100 ml of dioxane brought to 80° C. The mixture is heated for a further 20 minutes after the addition is complete. The reaction mixture is filtered while hot in order to remove the inorganic salts. The expected product is precipitated by diluting the cooled filtrate with ice-cold water. When recrystallized from ethyl acetate, it melts at 190° C.

후처리

  1. custombrought to 80° C
  2. temperatureThe mixture is heated for a further 20 minutes
  3. additionafter the addition
  4. filtrationThe reaction mixture is filtered while hot in order
  5. customto remove the inorganic salts
  6. customThe expected product is precipitated
  7. additionby diluting the cooled filtrate with ice-cold water
  8. customWhen recrystallized from ethyl acetate, it melts at 190° C.

출처 및 근거

ORD 기록
ord-60c21051c95c458da80631cd1ff0e295
출처 데이터셋
uspto-grants-1992_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05145483

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