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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Sodium Chloride → HCID 13021078, 화합물

HRID 1446811
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HRID 1446811 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

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

생성물 1

HCID 13021078HCID 13021078, 화합물

시약·촉매·용매 2

HCID 6228Dimethylformamide용매
HCID 8028
Tetrahydrofuran
용매

실험 절차

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

후처리

  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

출처 및 근거

ORD 기록
ord-c715101eedd6491686439bafe3129280
출처 데이터셋
uspto-grants-1982_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04313950

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