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

Ethanolamine → HCID 19600009、化合物

HRID 611245
ノート
印刷プレビュー

反応式

HRID 611245 の反応式
[C:1]1([CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][C:12]([N:14]2[CH2:19][CH2:18][C:17]3[CH:20]=[C:21]([C:23]([OH:25])=O)[O:22][C:16]=3[CH2:15]2)=[O:13])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[NH2:26][CH2:27][CH2:28]O.C(N(CC)CC)C.C(Cl)(Cl)(Cl)Cl.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>C(#N)C.O>[O:25]1[CH2:28][CH2:27][N:26]=[C:23]1[C:21]1[O:22][C:16]2[CH2:15][N:14]([C:12](=[O:13])[CH2:11][CH2:10][CH2:9][CH2:8][CH2:7][C:1]3[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=3)[CH2:19][CH2:18][C:17]=2[CH:20]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 700EthanolamineHCID 5943Carbon TetrachlorideHCID 8471TriethylamineHCID 11776TriphenylphosphineHCID 19599954HCID 19599954、化合物

生成物 1

HCID 19600009HCID 19600009、化合物

試薬・触媒・溶媒 2

HCID 962
Water
溶媒
HCID 6342Acetonitrile溶媒

実験手順

To a solution of 0.884 g (2.590 mmol) of 6-(6-phenylhexanoyl)-4,5,6,7-tetrahydrofuro[2,3-c]pyridine-2-carboxylic acid, 0.16 g (2.59 mmol) of 2-aminoethanol, 1.08 ml (7.77 mmol) of triethylamine and 2.50 ml (25.9 mmol) of carbon tetrachloride in 50 ml of acetonitrile, 2.04 g (7.77 mmol) of triphenylphosphine was added under ice-cooling, followed by stirring at room temperature for 4 hours. The reaction mixture was poured into water and extracted with ethyl acetate 3 times. The combined organic layer was dried over anhydrous magnesium sulfate; the solvent was distilled off under reduced pressure. The resulting crude product was purified by silica gel flush column chromatography (ethyl acetate to ethyl acetate/methanol=20/1) to yield the desired product.

後処理

  1. temperaturecooling
  2. extractionextracted with ethyl acetate 3 times
  3. dry with materialThe combined organic layer was dried over anhydrous magnesium sulfate
  4. distillationthe solvent was distilled off under reduced pressure
  5. customThe resulting crude product was purified by silica gel
  6. customflush column chromatography (ethyl acetate to ethyl acetate/methanol=20/1)

出典と根拠

ORDレコード
ord-daa68a339bbb495d8a1f11eb25a0cf09
出典データセット
uspto-grants-1999_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05998433

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート