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

HRID 1885497
ノート
印刷プレビュー

反応式

HRID 1885497 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

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.

後処理

  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.

出典と根拠

ORDレコード
ord-b37f28bf79554056bc20012edc1a7fa2
出典データセット
uspto-grants-1992_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05145483

反応ノート

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