Hydrochloric Acid → 5-(2-chloroethylidene)-10,11-dihydro-5H-dibenzo[a,d]cycloheptene

HRID 865624노트

반응식

HRID 865624 반응식
[ClH:1].[CH2:2]=[C:3]1[C:9]2[CH:10]=[CH:11][CH:12]=[CH:13][C:8]=2[CH2:7][CH2:6][C:5]2[CH:14]=[CH:15][CH:16]=[CH:17][C:4]1=2.[CH2:18]=O>C(O)(=O)C>[Cl:1][CH2:18][CH:2]=[C:3]1[C:4]2[CH:17]=[CH:16][CH:15]=[CH:14][C:5]=2[CH2:6][CH2:7][C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][C:9]1=2

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 712FormaldehydeHCID 46413975-Methylene-10,11-dihydro-5H-dibenzo[a,d][7]annulene

생성물 1

HCID 124928075-(2-chloroethylidene)-10,11-dihydro-5H-dibenzo[a,d]cycloheptene

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

In the same manner as in (2) in Example 2, hydrogen chloride gas was bubbled into the mixture of 20.6 g (0.1 mol) of 10,11-dihydro-5-methylene-5H-dibenzo[a,d]cycloheptene (4c), 41 g of acetic acid, and 4.5 g (0.15 mol) of paraformaldehyde. After reaction was conducted, the reaction product was extracted with toluene, neutralized with a saturated sodium bicarbonate solution, and washed with water. Further, this product was dried with sodium sulfate anhydride, concentrated and then recrystallized from hexane to obtain 23.4 g of the compound (5c).

후처리

  1. customAfter reaction
  2. extractionthe reaction product was extracted with toluene
  3. washwashed with water
  4. dry with materialFurther, this product was dried with sodium sulfate anhydride
  5. concentrationconcentrated
  6. customrecrystallized from hexane

출처 및 근거

ORD 기록
ord-0e4b4f906d1c446dad3f7a638fb8f715
출처 데이터셋
uspto-grants-1996_10
특허 번호
US05567560

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