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Potassium Iodide → HCID 18982209, 화합물

HRID 1440819
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HRID 1440819 반응식
[Cl:1][CH2:2][CH2:3][O:4][C:5]1[C:14]2[O:13][CH2:12][CH2:11][O:10][C:9]=2[CH:8]=[CH:7][CH:6]=1.Br.[F:16][C:17]1[CH:31]=[CH:30][C:20]([C:21]([CH:23]2[CH2:29][CH2:28][CH2:27][NH:26][CH2:25][CH2:24]2)=[O:22])=[CH:19][CH:18]=1.[I-].[K+].C(=O)([O-])[O-].[K+].[K+]>C(C(CC)=O)C.CC(C)=O.CCOCC.CO>[ClH:1].[F:16][C:17]1[CH:18]=[CH:19][C:20]([C:21]([CH:23]2[CH2:29][CH2:28][CH2:27][N:26]([CH2:2][CH2:3][O:4][C:5]3[C:14]4[O:13][CH2:12][CH2:11][O:10][C:9]=4[CH:8]=[CH:7][CH:6]=3)[CH2:25][CH2:24]2)=[O:22])=[CH:30][CH:31]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 4875Potassium IodideHCID 11430Potassium CarbonateHCID 114699561,4-Benzodioxin, 5-(2-chloroethoxy)-2,3-dihydro-HCID 18982196HCID 18982196, 화합물

생성물 1

HCID 18982209HCID 18982209, 화합물

시약·촉매·용매 3

HCID 887Methanol용매
HCID 7288
Ethyl ketone
용매
HCID 21584533Acetone diethylether용매

실험 절차

A mixture of 5 g of 5-(2-chloroethoxy)-1,4-benzodioxane, 7.8 g of 4-(4-fluorobenzoyl)perhydroazepine hydrobromide (described in Patent EP 389,352), 1 g of potassium iodide and 6.5 g of potassium carbonate in 100 ml of diethyl ketone is maintained at 100 C. for 24 hours. The inorganic salts are then filtered off and the filtrate is concentrated under vacuum. The residue is purified by chromatography on a column of silica, with a dichloromethane/methanol/aqueous ammonia (97/3/0.3) eluent mixture. The base obtained is salified with hydrochloric methanol in an acetone/ether mixture. Melting point: 106°-107° C.

후처리

  1. temperatureis maintained at 100 C
  2. filtrationThe inorganic salts are then filtered off
  3. concentrationthe filtrate is concentrated under vacuum
  4. customThe residue is purified by chromatography on a column of silica, with a dichloromethane/methanol/aqueous ammonia (97/3/0.3) eluent mixture
  5. customThe base obtained

출처 및 근거

ORD 기록
ord-0d2c21b63c4a43dab9d4913c9d180fc0
출처 데이터셋
uspto-grants-1996_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05500443

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