Phenothiazine → Phenothiazine-10-propionitrile

HRID 364914

반응식

HRID 364914 반응식
[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]

참가 물질

7

반응물 4

HCID 7108PhenothiazineHCID 7855Acrylonitrile2회HCID 64819Antioxidant 10102회HCID 66854Benzyltrimethylammonium hydroxide

생성물 1

HCID 228554Phenothiazine-10-propionitrile

시약·촉매·용매 2

HCID 180Acetone용매HCID 6342Acetonitrile용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-0f1b3735b74a4b36b06d6a4189be648a
출처 데이터셋
uspto-grants-1986_08
특허 번호
US04607006

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