ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Phosgene → HCID 11003433、化合物

HRID 742092
ノート
印刷プレビュー

反応式

HRID 742092 の反応式
[NH:1]1[CH:5]=[N:4][CH:3]=[N:2]1.[O:6]([C:13]1[CH:18]=[CH:17][C:16]([C:19]([CH3:26])([OH:25])[C:20]([O:22][CH2:23][CH3:24])=[O:21])=[CH:15][CH:14]=1)[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1.N1C=CN=N1.[C:32](Cl)(Cl)=[O:33]>C(N(CC)CC)C.C1(C)C=CC=CC=1>[N:1]1([C:32]([O:25][C:19]([CH3:26])([C:16]2[CH:17]=[CH:18][C:13]([O:6][C:7]3[CH:8]=[CH:9][CH:10]=[CH:11][CH:12]=3)=[CH:14][CH:15]=2)[C:20]([O:22][CH2:23][CH3:24])=[O:21])=[O:33])[CH:5]=[N:4][CH:3]=[N:2]1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 6371PhosgeneHCID 92571H-1,2,4-TriazoleHCID 10859095Ethyl 2-(4-phenoxyphenyl)lactateHCID 178418936HCID 178418936、化合物

生成物 1

HCID 11003433HCID 11003433、化合物収率 102.9%

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒
HCID 8471
Triethylamine
溶媒

反応条件

温度
103 °C

実験手順

A mixture of 6.9 g of 1,2,4-triazole, 100 mL of toluene, 14.3 g of ethyl 2-(4phenoxyphenyl)lactate, and 20 g of triethylamine was heated to 103° C. to dissolve the triazole and then cooled to -60° C. Phosgene (6.4 g) was added at 57°-60° C. over 2.5 h. After holding the reaction mixture at 59°-60° C. for 1.25 h, the reaction mixture was cooled to -5° C. Ice (100 g) was added, and the temperature dropped to -8° C. The aqueous layer was separated and extracted one time with 15 mL of toluene. The organic layers were combined and washed with cold water (2 times with 25 mL), dried (MgSO4), filtered, and evaporated in vacuo to yield 19.6 g of the title compound as a viscous oil. 1H NMR (300 MHz, CDCl3): δ8.85 (s, 1H), 8.08 (s,1H), 7.59-7.00 (m, 11H), 4.25 (m,2H), 2.18 (s,3H), 1.23 (t,3H).

後処理

  1. temperaturecooled to -60° C
  2. customat 59°-60° C.
  3. customfor 1.25 h
  4. temperaturethe reaction mixture was cooled to -5° C
  5. additionthe temperature dropped to -8° C
  6. customThe aqueous layer was separated
  7. extractionextracted one time with 15 mL of toluene
  8. washwashed with cold water (2 times with 25 mL)
  9. dry with materialdried (MgSO4)
  10. filtrationfiltered
  11. customevaporated in vacuo

出典と根拠

ORDレコード
ord-a71173dd1f1f4e23b635a9b145ddd388
出典データセット
uspto-grants-1996_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05552554

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート