Phenothiazine → Phenothiazine-10-propionitrile

HRID 2413671

反応式

HRID 2413671 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

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 180Acetone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 relfuxing 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.

後処理

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

出典と根拠

ORDレコード
ord-b16c8f8121544235aa15044c9676186c
出典データセット
uspto-grants-1988_01
特許番号
US04719174

関連ノート

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