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Dimethylformamide → HCID 68128747, 화합물

HRID 1077049
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HRID 1077049 반응식
[CH2:1]1[C:11]2[N:10]3[C:12]4[CH:21]=[CH:20][N:19]=[CH:18][C:13]=4[C:14]4[CH2:15][CH2:16][CH:17]=[C:8]([C:9]=43)[CH:7]=[CH:6][C:5]=2[CH2:4][CH2:3][CH2:2]1.Br[CH2:23][CH:24]=[CH2:25].C(=O)(O)[O-].[Na+].CN(C)C=O>O>[CH2:25]([CH:3]1[CH2:4][C:5]2[CH:6]=[CH:7][C:8]3[C:9]4[N:10]([C:12]5[CH:21]=[CH:20][N:19]=[CH:18][C:13]=5[C:14]=4[CH2:15][CH2:16][CH:17]=3)[C:11]=2[CH2:1][CH2:2]1)[CH:24]=[CH2:23]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 7841Allyl bromideHCID 516892Sodium BicarbonateHCID 67838308HCID 67838308, 화합물

생성물 1

HCID 68128747HCID 68128747, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of 3.3 g. of the product of Example 1, 1.45 g. of freshly distilled 3-bromopropene and 1.7 g. of sodium bicarbonate is stirred at room temperature, for 24 hours, in 50 ml. dimethylformamide. At the end of this period, the mixture is poured into water, extracted with ether, and the combined extracts are dried and stripped down. The residue is dissolved in benzene, and the resulting solution chromatographed through a column of neutral alumina. The oily residue obtained on stripping down the eluate is recrystallized from isopropyl alcohol to yield 3-allyl-1,2,3,4,8,9-hexahydropyrido[4',3':2,3]indolo[1,7-ab][1]benzazepine m.p. 112°-113°.

후처리

  1. additionA mixture of 3.3 g
  2. extractionextracted with ether
  3. customthe combined extracts are dried
  4. dissolutionThe residue is dissolved in benzene
  5. customthe resulting solution chromatographed through a column of neutral alumina
  6. customThe oily residue obtained
  7. customis recrystallized from isopropyl alcohol

출처 및 근거

ORD 기록
ord-067d6eb5f37344f69c32f58c564d32ca
출처 데이터셋
uspto-grants-1976_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03959300

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