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Triethanolamine → HCID 178506208、化合物

HRID 2075119
ノート
印刷プレビュー

反応式

HRID 2075119 の反応式
[Cl:1][C:2]1[CH:26]=[CH:25][C:24]([C:27]([F:30])([F:29])[F:28])=[CH:23][C:3]=1[CH2:4][N:5]([CH2:8][C:9]1[CH:14]=[C:13]([C:15]([F:18])([F:17])[F:16])[CH:12]=[C:11]([C:19]([F:22])([F:21])[F:20])[CH:10]=1)[C:6]#[N:7].N(CCO)(CCO)CCO.C[Si]([N:45]=[N+:46]=[N-:47])(C)C>[OH-].[Na+]>[Cl:1][C:2]1[CH:26]=[CH:25][C:24]([C:27]([F:28])([F:29])[F:30])=[CH:23][C:3]=1[CH2:4][N:5]([CH2:8][C:9]1[CH:10]=[C:11]([C:19]([F:20])([F:21])[F:22])[CH:12]=[C:13]([C:15]([F:18])([F:17])[F:16])[CH:14]=1)[C:6]1[NH:47][N:46]=[N:45][N:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 7618TriethanolamineHCID 78378AzidotrimethylsilaneHCID 86614965(2-Chloro-5-(trifluoromethyl)benzyl)(3,5-bis(trifluoromethyl)benzyl)cyanamide

生成物 1

HCID 178506208HCID 178506208、化合物収率 85%

試薬・触媒・溶媒 1

HCID 14798Sodium Hydroxide溶媒

実験手順

A solution of 5 gm of the compound from Step C, 50 mL of 2-methyl THF 5 mL, triethanolamine and 2.5 mL of trimethyl silyl azide was heated at 50° C. until reaction completion. When the reaction was judged complete, the reaction mixture was cooled and 50 mL of 1 N sodium hydroxide added, The layers were separated and the organic layer washed with 50 mL of 10% citric acid. The organic layer was concentrated and triturated with hexane to yield 4.6 of the desired compound. 85% yield. 1H NMR (400 MHz, CDCl3) 7.84 (s, 2H), 7.74 (m, 3H), 4.90 (s, 4H)C, H, N, Calculated, (found) 42.92 (42.98), 2.20 (1.97), 13.90 (13.54)

後処理

  1. temperaturethe reaction mixture was cooled
  2. customThe layers were separated
  3. washthe organic layer washed with 50 mL of 10% citric acid
  4. concentrationThe organic layer was concentrated
  5. customtriturated with hexane

出典と根拠

ORDレコード
ord-499a530ea3b64abe8a62d4e497961329
出典データセット
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07919506B2

反応ノート

読み込み中…

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