Sodium Hydroxide → TK 12997

HRID 435223

反応式

HRID 435223 の反応式
[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

参加物

5

反応物 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

生成物 1

HCID 163462TK 12997収率 80.3%

試薬・触媒・溶媒 1

HCID 7237O-Xylene溶媒

反応条件

温度
25 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-ab798ed61532423db0058180fe16f7d9
出典データセット
uspto-grants-1983_08
特許番号
US04400505

関連ノート

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