Malononitrile → HCID 54446985, 화합물

HRID 616497노트

반응식

HRID 616497 반응식
C(N(CC)CC)C.[C:8](#[N:12])[CH2:9][C:10]#[N:11].[Cl-].Cl[C:15]([Cl:21])=[N+:16]([CH2:19][CH3:20])[CH2:17][CH3:18]>ClC1C=CC=CC=1>[Cl:21][C:15]([N:16]([CH2:17][CH3:18])[CH2:19][CH3:20])=[C:9]([C:8]#[N:12])[C:10]#[N:11]

참가 물질

5

반응물 3

HCID 8010MalononitrileHCID 8471TriethylamineHCID 12331502Dichloro-N,N-diethylmethaniminium chloride

생성물 1

HCID 54446985HCID 54446985, 화합물수율 33.7%

시약·촉매·용매 1

HCID 7964Chlorobenzene용매2회

실험 절차

A solution of 12.1 g of triethylamine, 4.0 g of malononitrile, and 20 ml of chlorobenzene was added to a slurry of 11.4 g of N-(dichloromethylene)-N,N-diethylammonium chloride and 50 ml of chlorobenzene, at ambient temperature. The reaction temperature was kept below 50° by controlling the rate of addition (time required for complete addition, 30 minutes). After addition, the reaction mixture was stirred for four hours while it returned to ambient temperature. The reaction mixture was filtered and the filtrate concentrated on the rotary evaporator to give a brownish-red liquid. Vacuum distillation gave 3.7 g of liquid 3-chloro-2-cyano-3-(diethylamino)propenenitrile; b.p. 127°-131°/0.05 mm Hg. The ir and nmr spectra were consistent with the assigned structure.

후처리

  1. customwas kept below 50°
  2. additionthe rate of addition (time required for complete addition, 30 minutes)
  3. additionAfter addition
  4. customreturned to ambient temperature
  5. filtrationThe reaction mixture was filtered
  6. concentrationthe filtrate concentrated on the rotary evaporator
  7. customto give a brownish-red liquid
  8. distillationVacuum distillation

출처 및 근거

ORD 기록
ord-f5cc1e970d8f47a9b4e12466066e45f1
출처 데이터셋
uspto-grants-1978_02
특허 번호
US04075001

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