Hexane → HCID 14835954, 화합물

HRID 1461285노트

반응식

HRID 1461285 반응식
[CH3:1][C:2]1[CH:3]=[N:4][C:5]2[CH2:6][CH2:7][CH2:8][CH2:9][C:10]=2[CH:11]=1.C([Li])CCC.CCCCCC.[C:23]1([Se:29]Cl)[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1>O1CCCC1.O>[CH3:1][C:2]1[CH:3]=[N:4][C:5]2[CH:6]([Se:29][C:23]3[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=3)[CH2:7][CH2:8][CH2:9][C:10]=2[CH:11]=1

참가 물질

7

반응물 4

HCID 8058HexaneHCID 21928ChloroselenobenzeneHCID 1200283-Methyl-5,6,7,8-tetrahydroquinolineHCID 178418339Butyllithium

생성물 1

HCID 14835954HCID 14835954, 화합물수율 98.6%

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매2회

실험 절차

A solution of 5,6,7,8-tetrahydro 3 methylquinoline (7.5 g, 51 mmol) in tetrahydrofuran (100 ml) was treated under an atmosphere of nitrogen with 1.5M-butyllithium in hexane (35 ml, 52 mmol) at 0°. The resulting red solution was added to a solution of phenylselenyl chloride (10 g, 52 mmol) in tetrahydrofuran (50 ml) at 0°. After 30 min, water (100 ml) was added and the mixture concentrated in vacuo. The aqueous residue was partitioned between saturated aqueous sodium chloride (100 ml) and ether (100 ml). The organic phase was dried (Na2SO4) and evaporated in vacuo to give the crude product (15.2 g) as an oil.

후처리

  1. concentrationthe mixture concentrated in vacuo
  2. customThe aqueous residue was partitioned between saturated aqueous sodium chloride (100 ml) and ether (100 ml)
  3. dry with materialThe organic phase was dried (Na2SO4)
  4. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-c4236ae4f3ae4394a84935f10227ef7a
출처 데이터셋
uspto-grants-1991_12
특허 번호
US05075303

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