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Phenothiazine → Phenothiazine-10-propionitrile

HRID 364914
ノート
印刷プレビュー

反応式

HRID 364914 の反応式
[OH-].[CH2:2]([N+:9](C)(C)C)[C:3]1C=CC=C[CH:4]=1.[CH:13]1[C:26]2[NH:25][C:24]3[C:19](=[CH:20][CH:21]=[CH:22][CH:23]=3)[S:18][C:17]=2[CH:16]=[CH:15][CH:14]=1.C(#N)C=C.CC(C1C(O)=C(C(C)(C)C)C=C(CCC(OCC(COC(CCC2C=C(C(C)(C)C)C(O)=C(C(C)(C)C)C=2)=O)(COC(CCC2C=C(C(C)(C)C)C(O)=C(C(C)(C)C)C=2)=O)COC(CCC2C=C(C(C)(C)C)C(O)=C(C(C)(C)C)C=2)=O)=O)C=1)(C)C>CC(C)=O.C(#N)C>[C:2]([CH2:3][CH2:4][N:25]1[C:26]2[CH:13]=[CH:14][CH:15]=[CH:16][C:17]=2[S:18][C:19]2[C:24]1=[CH:23][CH:22]=[CH:21][CH:20]=2)#[N:9]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 7108PhenothiazineHCID 7855Acrylonitrile2 回HCID 64819Antioxidant 10102 回HCID 66854Benzyltrimethylammonium hydroxide

生成物 1

HCID 228554Phenothiazine-10-propionitrile

試薬・触媒・溶媒 2

HCID 180
Acetone
溶媒
HCID 6342Acetonitrile溶媒

実験手順

4 ml of Triton B (40%) (benzyltrimethylammonium hydroxide) was dropwise added to an acetonitrile solution (200 ml) containing 199 g of phenothiazine, 106 g of acrylonitrile, and a small quantity of Irganox 1010 (made by Ciba Geigy Co.). Irganox 1010 has the formula ##STR4## After refluxing for 3 hours while heating, 53 g of acrylonitrile was added thereto, followed by refluxing for a further 2 hours while heating. After being allowed to cool, acetone was added to the reaction solution to crystallize the reaction product. Crystals thus formed were collected by filtration, and recrystallized from 900 ml of acetone to obtain 135 g of the desired compound. m.p. 158°-160° C.

後処理

  1. temperature##STR4## After refluxing for 3 hours
  2. temperaturewhile heating
  3. temperatureby refluxing for a further 2 hours
  4. temperaturewhile heating
  5. temperatureto cool
  6. customto crystallize the reaction product
  7. customCrystals thus formed
  8. filtrationwere collected by filtration
  9. customrecrystallized from 900 ml of acetone

出典と根拠

ORDレコード
ord-0f1b3735b74a4b36b06d6a4189be648a
出典データセット
uspto-grants-1986_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04607006

反応ノート

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