(1,4-Phenylenebis(methylene))bis(triphenylphosphonium) dibromide → 1,1'-[1,4-Phenylenedi(ethene-2,1-diyl)]bis[4-(pentadecyloxy)benzene]

HRID 1863831

반응식

HRID 1863831 반응식
[CH2:1]([O:16][C:17]1[CH:24]=[CH:23][C:20]([CH:21]=O)=[CH:19][CH:18]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH3:15].C1C=CC([P+](C2C=CC=CC=2)(C2C=CC=CC=2)[CH2:32][C:33]2[CH:38]=[CH:37][C:36]([CH2:39][P+](C3C=CC=CC=3)(C3C=CC=CC=3)C3C=CC=CC=3)=[CH:35][CH:34]=2)=CC=1.[Br-].[Br-]>CO>[CH2:1]([O:16][C:17]1[CH:24]=[CH:23][C:20]([CH:21]=[CH:39][C:36]2[CH:35]=[CH:34][C:33]([CH:32]=[CH:21][C:20]3[CH:23]=[CH:24][C:17]([O:16][CH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH3:15])=[CH:18][CH:19]=3)=[CH:38][CH:37]=2)=[CH:19][CH:18]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH3:15]

참가 물질

4

반응물 2

HCID 2723797(1,4-Phenylenebis(methylene))bis(triphenylphosphonium) dibromideHCID 23127399p-Pentadecanoxybenzaldehyde

생성물 1

HCID 579729461,1'-[1,4-Phenylenedi(ethene-2,1-diyl)]bis[4-(pentadecyloxy)benzene]수율 92.9%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A 30-ml four-necked flask was used, 7.87 g (23.7 mM) of p-pentadecanoxybenzaldehyde synthesized as described above and 8.65 g (11.0 mM) of p-xylylenebis(triphenylphosphonium bromide) were suspended in 100 ml of methanol, and 6.87 g (35.6 mM) of 28-percent by weight methylate was dropped thereto at room temperature (25° C.). Thereafter, aging was performed at a reflux temperature of 65° C. for 3 hours. Methanol was distilled out, and 200 ml of water was added to the residue, followed by agitation. Subsequently, the precipitate was filtrated. The resulting precipitate was further washed with water and acetone, followed by drying, so as to produce 7.49 g of 1,4-bis(4′-pentadecanoxystyryl)benzene isomer mixture (Compound (7)).

후처리

  1. customA 30-ml four-necked flask was used
  2. addition6.87 g (35.6 mM) of 28-percent by weight methylate was dropped
  3. customat room temperature
  4. custom(25° C.)
  5. distillationMethanol was distilled out
  6. addition200 ml of water was added to the residue
  7. filtrationSubsequently, the precipitate was filtrated
  8. washThe resulting precipitate was further washed with water and acetone
  9. customby drying

출처 및 근거

ORD 기록
ord-28e86a10ab5f40e7a68ea9e22227d7fa
출처 데이터셋
uspto-grants-2009_12
특허 번호
US07625499B2

연결된 노트

불러오는 중…