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Phosphoric Acid → HCID 22810374, 화합물

HRID 1390108
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HRID 1390108 반응식
[O:1]([C:8]1[CH:26]=[CH:25][C:11]([CH2:12][CH:13]2[C:22]3[CH2:21][CH2:20][CH2:19][CH2:18][C:17]=3[CH2:16][CH2:15][N:14]2[CH:23]=[O:24])=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.P(=O)(O)(O)O.S(=O)(=O)(O)O>>[O:1]([C:8]1[CH:9]=[CH:10][C:11]2[CH2:12][C@H:13]3[N:14]([CH:23]=[O:24])[CH2:15][CH2:16][C@@:17]4([C:25]=2[CH:26]=1)[C@H:22]3[CH2:21][CH2:20][CH2:19][CH2:18]4)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 1004Phosphoric AcidHCID 1118Sulfuric AcidHCID 12876713HCID 12876713, 화합물

생성물 1

HCID 22810374HCID 22810374, 화합물수율 95%

실험 절차

(±)-1-(p-Phenoxybenzyl)-2-formyl-1,2,3,4,5,6,7,8-octahydroisoquinoline, 24.5 g (0.07 mol), was combined under stirring with 120 g of phosphoric acid which had been mixed with 1.0 g of concentrated sulfuric acid and the mixture was heated in a nitrogen atmosphere to 70°. The resulting homogeneous solution was kept at 70° for 48 hrs. The mixture was cooled in an ice bath and ice-water was added. The resulting suspension was extracted with ethyl acetate (100 ml). The ethyl acetate solution was washed with water and dried. Removal of the solvent gave 23.3 g (95%) of crude (±)-3-phenoxy-N-formylmorphinan.

후처리

  1. temperaturethe mixture was heated in a nitrogen atmosphere to 70°
  2. temperatureThe mixture was cooled in an ice bath
  3. extractionThe resulting suspension was extracted with ethyl acetate (100 ml)
  4. washThe ethyl acetate solution was washed with water
  5. customdried
  6. customRemoval of the solvent

출처 및 근거

ORD 기록
ord-a63417150c19498eb4d3c5ae59672ef8
출처 데이터셋
uspto-grants-1981_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04247697

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