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Sodium Chloride → HCID 13021078、化合物

HRID 1446811
ノート
印刷プレビュー

反応式

HRID 1446811 の反応式
[NH2:1]OS(=O)=O.[H-].[Na+].[C:8]1(=[O:19])[C:14]2[CH:15]=[CH:16][CH:17]=[CH:18][C:13]=2[CH2:12][CH2:11][CH2:10][NH:9]1.[Na+].[Cl-]>CN(C)C=O.O1CCCC1>[NH2:1][N:9]1[CH2:10][CH2:11][CH2:12][C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=2[C:8]1=[O:19]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 5234Sodium ChlorideHCID 24758Sodium hydrideHCID 112406552,3,4,5-tetrahydro-1H-2-benzazepin-1-oneHCID 178514657HCID 178514657、化合物

生成物 1

HCID 13021078HCID 13021078、化合物

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒
HCID 8028
Tetrahydrofuran
溶媒

実験手順

A solution of 2.7 g of O-amino-sulfonic acid and 1.25 g of a 55% oily suspension of sodium hydride in 30 ml of dimethylformamide and 30 ml of tetrahydrofuran was gradually added at a temperature of 10° C. to a suspension of 9.66 g (0.0176 mol) 4,5-dihydro-2-benzazepine-1(2H,3H)-one. After standing for 1 hour at room temperature the mixture was poured into a saturated aqueous solution of NaCl, then the organic layer was separated and the mother liquors were extracted with 300 ml (3×100 ml) of an 1:1 (v:v) mixture of tetrahydrofuran and dimethylformamide. The organic phases were combined and brought to dryness. The obtained residue was subsequently taken up with 500 ml of ethyl acetate and the resulting organic solution was extracted with 200 ml (5×40 ml) of a 3% aqueous solution of HCl. The acidic extract was made alkaline with 5% aqueous sodium hydroxide and subsequently extracted with ethyl acetate. After evaporating the solvent, an oily residue was obtained which was distilled under reduced pressure. Yield: 10 g. of the title compound. B.p. 120° C./0.2 mmHg

後処理

  1. customthe organic layer was separated
  2. extractionthe mother liquors were extracted with 300 ml (3×100 ml) of an 1:1 (v:v) mixture of tetrahydrofuran and dimethylformamide
  3. extractionthe resulting organic solution was extracted with 200 ml (5×40 ml) of a 3% aqueous solution of HCl
  4. extractionThe acidic extract
  5. extractionsubsequently extracted with ethyl acetate
  6. customAfter evaporating the solvent
  7. customan oily residue was obtained which
  8. distillationwas distilled under reduced pressure

出典と根拠

ORDレコード
ord-c715101eedd6491686439bafe3129280
出典データセット
uspto-grants-1982_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04313950

反応ノート

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