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Dichloromethane → HCID 70633015, 화합물

HRID 329017
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HRID 329017 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.ClCCl.[CH:25]1([C:28](Cl)=[O:29])[CH2:27][CH2:26]1>C(N(CC)CC)C>[CH:25]1([C:28]([CH:3]2[CH2:4][C:5]3[CH:6]=[CH:7][C:8]4[C:9]5[N:10]([C:12]6[CH:21]=[CH:20][N:19]=[CH:18][C:13]=6[C:14]=5[CH2:15][CH2:16][CH:17]=4)[C:11]=3[CH2:1][CH2:2]2)=[O:29])[CH2:27][CH2:26]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6344DichloromethaneHCID 77637Cyclopropanecarbonyl chlorideHCID 67838308HCID 67838308, 화합물

생성물 1

HCID 70633015HCID 70633015, 화합물

시약·촉매·용매 1

HCID 8471Triethylamine용매

실험 절차

To a solution of 16.4 g of 1,2,3,4,8,9-hexahydropyrido[4',3':2,3]indolo[1,7-ab][1]benzazepine in 500 ml. of dichloromethane, 7.3 g. of cyclopropanecarbonyl chloride was added, followed by dropwise addition of 10 ml. of triethylamine. A mildly exothermic reaction took place, after which stirring of the mixture was continued at room temperature overnight. The mixture was then washed with 1N hydrochloric acid and water and dried over anhydrous sodium carbonate. On evaporation to dryness, crude 3-(cyclopropylcarbonyl)-1,2,3,4,8,9-hexahydropyrido[4',3':2,3]indolo[1,7-ab][1]benzazepine was obtained as a glassy product. Recrystallization from ethanol yielded the pure material, m.p. 154°-156° C.

후처리

  1. additionfollowed by dropwise addition of 10 ml
  2. customA mildly exothermic reaction
  3. washThe mixture was then washed with 1N hydrochloric acid and water
  4. dry with materialdried over anhydrous sodium carbonate
  5. customOn evaporation to dryness

출처 및 근거

ORD 기록
ord-75f48ae26de445fc93ebe9fb80d13cb3
출처 데이터셋
uspto-grants-1977_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04018930

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