Glycol monoethyl ether → HCID 178492518, 화합물

HRID 1833517노트

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HRID 1833517 반응식
C(OCCO)C.[S-2].[Na+].[Na+].[Na].[CH3:11][O:12][C:13]1[CH:21]=[CH:20][C:19]([O:22][CH3:23])=[C:18]2[C:14]=1[CH:15](S)[NH:16][C:17]2=[NH:24].C1(S([O-])(=O)=O)C=CC=CC=1.[NH:36]=[C:37]1[NH2+:41][C:40](=[NH:42])[CH2:39][S:38]1>>[CH3:11][O:12][C:13]1[CH:21]=[CH:20][C:19]([O:22][CH3:23])=[C:18]2[C:14]=1[C:15](=[C:39]1[S:38][C:37](=[NH:36])[NH:41][C:40]1=[NH:42])[NH:16][C:17]2=[NH:24]

참가 물질

6

반응물 5

HCID 8076Glycol monoethyl etherHCID 14804Sodium SulfideHCID 5360545SodiumHCID 867342112,4-Diiminothiazolidinium benzenesulfonateHCID 178492520HCID 178492520, 화합물

생성물 1

HCID 178492518HCID 178492518, 화합물

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온도
25 °C

실험 절차

To 140 parts of 2-ethoxyethanol stirred at 100° C under an atmosphere of nitrogen there was added 8.6 parts of 60 percent active solid sodium sulfide and the resultant solution was filtered to remove undissolved material. The filtrate was mixed with 94 parts of dimethylformamide and 11.3 parts of 3,6-dimethoxy-phthalonitrile nd the mixture stirred at 25° C for a period of one hour. The reaction mixture was then heated to 95° C over a period of 1 hour, cooled to 25° C and filtered to remove undissolved material which was found to be (4.5 parts) unreacted 3,6-dimethoxyphthalonitrile. The filtrate, which contained approximately 0.04 mole of the sodium salt of 4,7-dimethoxy-1-imino-3-mercaptoisoindoline was stirred and there as added 10.7 parts of 2,4-diiminothiazolidinium benzenesulfonate. Stirring was continued overnight at 25° C. The product which separated was collected by filtration, washed successively with four portions of 12.0 parts each of methyl alcohol and finally dried in vacuo to obtain 4.5 parts of 4,7-dimethoxy-1-imino-3-(2,4-diimino-5-thiazolidinylidene)isoindoline as a red solid which melted at 227°-246° C (dec).

후처리

  1. filtrationthe resultant solution was filtered
  2. customto remove undissolved material
  3. additionThe filtrate was mixed with 94 parts of dimethylformamide and 11.3 parts of 3,6-dimethoxy-phthalonitrile nd the mixture
  4. temperatureThe reaction mixture was then heated to 95° C over a period of 1 hour
  5. temperaturecooled to 25° C
  6. filtrationfiltered
  7. customto remove undissolved material which
  8. stirringwas stirred
  9. stirringStirring
  10. waitwas continued overnight at 25° C
  11. customThe product which separated
  12. filtrationwas collected by filtration
  13. washwashed successively with four portions of 12.0 parts each of methyl alcohol
  14. customfinally dried in vacuo

출처 및 근거

ORD 기록
ord-b12d6b10e5404adbb1dc3e3afa4d2fcc
출처 데이터셋
uspto-grants-1978_01
특허 번호
US04066653

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