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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Allyl chloride → Allyl chloride

HRID 354598
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HRID 354598 반응식
BrC1C(Br)=C(Br)C(Br)=[C:6]2[C:11](=O)OC(=O)[C:7]=12.C(=O)([O-])[O-].[Na+].[Na+].[OH-].[Na+].[Na].BrC1C(Br)=C(Br)C(Br)=C(C([O-])=O)C=1C(OCC=C)=O.[CH2:44]([Cl:47])[CH:45]=[CH2:46].[CH2:48]([N:50]([CH2:53][CH3:54])[CH2:51][CH3:52])[CH3:49]>C(O)C=C>[CH2:44]([Cl:47])[CH:45]=[CH2:46].[Cl-:47].[CH2:11]([N+:50]([CH2:53][CH3:54])([CH2:51][CH3:52])[CH2:48][CH3:49])[CH:6]=[CH2:7]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

10

반응물 7

HCID 7850Allyl chlorideHCID 8471Triethylamine2회HCID 10340Sodium CarbonateHCID 12443Tetrabromophthalic anhydride2회HCID 14798Sodium Hydroxide2회HCID 5360545SodiumHCID 20508441Monoallyl tetrabromophthalate

생성물 2

HCID 7850Allyl chlorideHCID 15376696Allyltriethylammonium chloride

시약·촉매·용매 1

HCID 7858Allyl Alcohol용매2회

실험 절차

In the preferred embodiment of this invention for the production of DATBP, 1 mole of tetrabromophthalic anhydride, 0.55 mole of sodium carbonate (or 1 mole of sodium hydroxide) and a catalytic amount (0.024 mole) of triethylamine are added to a large excess (up to 10-20 moles) of allyl alcohol as a solvent as well as a reactant. If sodium hydroxide is used as the base, it is convenient to dissolve it in the allyl alcohol before the addition of the tetrabromophthalic anhydride. The mixture is stirred and heated to 90° C.-95° C. to speed the reaction to completion, yielding a solution or a thin suspension of the sodium salt of monoallyl tetrabromophthalate. After the completion of this step, 1.2 moles of allyl chloride plus a catalytic amount (0.33 mole) of allyltriethylammonium chloride (either preformed or formed in situ from triethylamine and additional allyl chloride) are added and the mixture is heated in a closed vessel for 2 hours at 100° C.-110° C., developing an equilibrium pressure of 103 kPa-172 kPa (15-25 psig). Longer heating may be required if no pressure is allowed to develop. On cooling, the DATBP crystallizes and the separated product requires only washing with cold water and drying to assay 94% to 98%. The washing may be accomplished by merely spraying with water in a centrifuge.

후처리

  1. temperatureheated to 90° C.-95° C.
  2. customthe reaction to completion
  3. customyielding a solution

출처 및 근거

ORD 기록
ord-c9922d6df8be44648d6627e93b082f7b
출처 데이터셋
uspto-grants-1983_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04375551

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