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Benzoyl chloride → 2-(N-benzyloxycarbonylamino)-5-(N-benzylcarbonylamino)phenol

HRID 1885497
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HRID 1885497 반응식
[C:1](Cl)(=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[NH2:10][C:11]1[CH:12]=[CH:13][C:14]([NH:18][C:19]([O:21][CH2:22][C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)=[O:20])=[C:15]([OH:17])[CH:16]=1.[C:29](=O)([O-])[O-:30].[Ca+2]>O1CCOCC1>[CH2:22]([O:21][C:19]([NH:18][C:14]1[CH:13]=[CH:12][C:11]([NH:10][C:29]([CH2:1][C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=2)=[O:30])=[CH:16][C:15]=1[OH:17])=[O:20])[C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1
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참가 물질

5

반응물 3

HCID 7412Benzoyl chlorideHCID 10112Calcium CarbonateHCID 147457335-Amino-2-(benzyloxycarbonylamino)phenol

생성물 1

HCID 147457402-(N-benzyloxycarbonylamino)-5-(N-benzylcarbonylamino)phenol

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

12 g of benzoyl chloride are slowly added dropwise to 0.77 mole (20 g) of 5-amino-2-(benzyloxycarbonylamino)phenol (prepared in the 2nd stage of Example 1) and 12 g of calcium carbonate in 120 ml of dioxane brought to 80° C. The mixture is heated for a further 20 minutes after the addition is complete. The mixture is filtered while hot in order to remove the inorganic salts. The expected product is precipitated by diluting the filtrate with ice-cold water. When recrystallized from methoxyethanol, it melts at 252° C.

후처리

  1. custombrought to 80° C
  2. temperatureThe mixture is heated for a further 20 minutes
  3. additionafter the addition
  4. filtrationThe mixture is filtered while hot in order
  5. customto remove the inorganic salts
  6. customThe expected product is precipitated
  7. additionby diluting the filtrate with ice-cold water
  8. customWhen recrystallized from methoxyethanol, it melts at 252° C.

출처 및 근거

ORD 기록
ord-b37f28bf79554056bc20012edc1a7fa2
출처 데이터셋
uspto-grants-1992_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05145483

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