Sodium Hydroxide → TK 12997

HRID 435223

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HRID 435223 반응식
[NH:1]([CH:19]1[CH2:24][C:23]([CH3:26])([CH3:25])[NH:22][C:21]([CH3:28])([CH3:27])[CH2:20]1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][NH:8][CH:9]1[CH2:14][C:13]([CH3:16])([CH3:15])[NH:12][C:11]([CH3:18])([CH3:17])[CH2:10]1.Cl[C:30]1[N:35]=[C:34]([NH:36][C:37]([CH2:40][C:41](C)(C)C)(C)C)[N:33]=[C:32]([NH:45][C:46]([CH2:49][C:50](C)(C)C)(C)C)[N:31]=1.[OH-].[Na+]>C1(C)C(C)=CC=CC=1>[CH3:25][C:23]1([CH3:26])[CH2:24][CH:19]([N:1]([C:30]2[N:31]=[C:32]([NH:45][CH2:46][CH:49]=[CH2:50])[N:33]=[C:34]([NH:36][CH2:37][CH:40]=[CH2:41])[N:35]=2)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][N:8]([C:30]2[N:31]=[C:32]([NH:45][CH2:46][CH:49]=[CH2:50])[N:33]=[C:34]([NH:36][CH2:37][CH:40]=[CH2:41])[N:35]=2)[CH:9]2[CH2:14][C:13]([CH3:16])([CH3:15])[NH:12][C:11]([CH3:17])([CH3:18])[CH2:10]2)[CH2:20][C:21]([CH3:28])([CH3:27])[NH:22]1

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 934191,6-Bis(2,2,6,6-tetramethyl-4-piperidylamino)hexaneHCID 64308146-Chloro-N,N'-(1,1,3,3-tetramethylbutyl)-[1,3,5]triazine-2,4-diamine

생성물 1

HCID 163462TK 12997수율 80.3%

시약·촉매·용매 1

HCID 7237O-Xylene용매

반응 조건

온도
25 °C

실험 절차

A stirred mixture of 4,4'(hexamethylenediimino)bis(2,2,6,6-tetramethylpiperidine) (6.36 grams; 0.0161 mole), 2-chloro-4,6-bis(t-octylamino)-1,3,5-triazine (9.56 grams; 0.0322 mole), and powdered sodium hydroxide (1.29 grams; 0.0322 mole) in xylene (75 mls) is stirred and heated at reflux while removing water therein by means of a water trap. The reaction mixture is stirred and heated at reflux for 18 hours, cooled to 25° C., and treated with acetonitrile (200 mls). The reaction mixture is filtered to recover a precipitate, and the solid is washed successively with water and acetone, and dried to obtain 10.0 grams of product which melts at 208°-209° C. after recrystallization from xylene.

후처리

  1. temperatureheated
  2. temperatureat reflux
  3. customwhile removing water
  4. stirringThe reaction mixture is stirred
  5. temperatureheated
  6. temperatureat reflux for 18 hours
  7. additiontreated with acetonitrile (200 mls)
  8. filtrationThe reaction mixture is filtered
  9. customto recover a precipitate
  10. washthe solid is washed successively with water and acetone
  11. customdried

출처 및 근거

ORD 기록
ord-ab798ed61532423db0058180fe16f7d9
출처 데이터셋
uspto-grants-1983_08
특허 번호
US04400505

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