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Sulfuric Acid → HCID 12953543, 화합물

HRID 848428
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HRID 848428 반응식
[C:1]1([C:7]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)([CH:10]2[CH2:13][N:12]([CH:14]([CH3:16])[CH3:15])[CH2:11]2)[C:8]#N)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.S(=O)(=O)(O)[OH:24].[OH-:28].[Na+]>>[C:1]1([C:7]2([C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=3)[CH:10]([CH2:13][NH:12][CH:14]([CH3:16])[CH3:15])[CH2:11][O:28][C:8]2=[O:24])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 1118Sulfuric AcidHCID 14798Sodium HydroxideHCID 12822282HCID 12822282, 화합물

생성물 1

HCID 12953543HCID 12953543, 화합물

반응 조건

온도
130 °C

실험 절차

α,α-Diphenyl-α-(1-isopropyl-3-azetidinyl)acetonitrile (142 g.; 0.49 mole) was added to 500 g. of 70% sulfuric acid at 90°-100° C. The temperature was raised to 130° C. for 48 hours. The cooled mixture was poured onto ice and the cold mixture made basic by the addition of solid sodium hydroxide. The basic mixture was extracted with chloroform and the combined chloroform extracts dried over sodium sulfate and concentrated. The residual material was crystallized from an 80% isooctane- 20% isopropyl ether solution. The 4,5-dihydro-3,3-diphenyl-4-isopropylaminomethylfuran-2(3H)one weighed 105 g. (69.3%) and melted at 78°-80° C.

후처리

  1. customat 90°-100° C
  2. additionThe cooled mixture was poured onto ice
  3. extractionThe basic mixture was extracted with chloroform
  4. dry with materialthe combined chloroform extracts dried over sodium sulfate
  5. concentrationconcentrated
  6. customThe residual material was crystallized from an 80% isooctane- 20% isopropyl ether solution

출처 및 근거

ORD 기록
ord-b14c9c70793b42fb918c811f9570043d
출처 데이터셋
uspto-grants-1981_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04296037

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