Water → HCID 70533310, 화합물

HRID 435449노트

반응식

HRID 435449 반응식
[C:1]1([C:7]2[C:8]3[O:13][CH2:12][O:11][CH:10](O)[C:9]=3[CH:15]=[CH:16][C:17]=2[C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.O=S(Cl)[Cl:26].C(Cl)Cl.O>CCOCC.N1C=CC=CC=1>[C:1]1([C:7]2[C:8]3[O:13][CH2:12][O:11][CH:10]([Cl:26])[C:9]=3[CH:15]=[CH:16][C:17]=2[C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

참가 물질

7

반응물 4

HCID 962WaterHCID 6344DichloromethaneHCID 24386Thionyl ChlorideHCID 70532672HCID 70532672, 화합물

생성물 1

HCID 70533310HCID 70533310, 화합물

시약·촉매·용매 2

HCID 1049Pyridine용매HCID 3283Diethyl Ether용매2회

실험 절차

To a stirred solution of 11.6 g. (38 mmol) of 3,4-diphenylmethylenedioxybenzyl alcohol in ether (80 ml.) and pyridine (0.6 ml.) at 20° C. was added dropwise a solution of SOCl2 in ether (40 ml.). The mixture was cooled to 0°-5° C., and CH2Cl2 and water were added. The layers were separated, and the organic layer was washed with water and saturated aqueous NaCl, dried over MgSO4 and concentrated to dryness to yield 3,4-diphenylmethylenedioxybenzyl chloride (11.43 g.) as a colorless viscous oil: tlc (silica gel CH2Cl2 : Rf 0.8; ir (CCl4) no --OH--, nmr (CCl4) δ 4.34 (s, 2H), 6.74 (d,j=8) 2H, 6.67 (s, 1H), 7.1-7.6 (m, 10H). ##STR11##

후처리

  1. temperatureThe mixture was cooled to 0°-5° C.
  2. customThe layers were separated
  3. washthe organic layer was washed with water and saturated aqueous NaCl
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated to dryness

출처 및 근거

ORD 기록
ord-184d5f6240034e1bb527e37469b92536
출처 데이터셋
uspto-grants-1983_08
특허 번호
US04401676

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