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Tetrahydrofuran → Allyl 4-[alpha-methoxycarbonyl-(5,6,7,8-tetrahydro-5,5,8,8-tetramethyl-2-naphthyl)acetamido]benzoate

HRID 726468
ノート
印刷プレビュー

反応式

HRID 726468 の反応式
[NH2:1][C:2]1[CH:13]=[CH:12][C:5]([C:6]([O:8][CH2:9][CH:10]=[CH2:11])=[O:7])=[CH:4][CH:3]=1.C1COCC1.C(N(CC)CC)C.[CH3:26][O:27][C:28]([CH:30]([C:34]1[CH:43]=[CH:42][C:41]2[C:40]([CH3:45])([CH3:44])[CH2:39][CH2:38][C:37]([CH3:47])([CH3:46])[C:36]=2[CH:35]=1)[C:31](Cl)=[O:32])=[O:29]>O>[CH3:26][O:27][C:28]([CH:30]([C:34]1[CH:43]=[CH:42][C:41]2[C:40]([CH3:45])([CH3:44])[CH2:39][CH2:38][C:37]([CH3:47])([CH3:46])[C:36]=2[CH:35]=1)[C:31]([NH:1][C:2]1[CH:3]=[CH:4][C:5]([C:6]([O:8][CH2:9][CH:10]=[CH2:11])=[O:7])=[CH:12][CH:13]=1)=[O:32])=[O:29]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 8028TetrahydrofuranHCID 8471TriethylamineHCID 13075143Prop-2-en-1-yl 4-aminobenzoateHCID 53969402alpha-Methoxycarbonyl-(5,6,7,8-tetrahydro-5,5,8,8-tetramethyl-2-naphthyl)acetic acid chloride

生成物 1

HCID 70275216Allyl 4-[alpha-methoxycarbonyl-(5,6,7,8-tetrahydro-5,5,8,8-tetramethyl-2-naphthyl)acetamido]benzoate

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

1.8 g (10 mmol) of allyl 4-aminobenzoate, 50 ml of THF and 1.7 ml (12 mmol) of triethylamine were introduced into a round-bottomed flask. A solution of 3.3 g (10 mmol) of α-methoxycarbonyl-(5,6,7,8-tetrahydro-5,5,8,8-tetramethyl-2-naphthyl)acetic acid chloride in 25 ml of THP was added dropwise and the mixture was stirred at room temperature for 2 hours. The reaction medium was poured into water, and extracted with ethyl acetate. The organic phase was decanted off, dried over magnesium sulfate and evaporated. The residue obtained was recrystallized from ethanol; 3.3 g (69%) of the expected compound of melting point 155°-156° C. were recovered after filtration and drying.

後処理

  1. extractionextracted with ethyl acetate
  2. customThe organic phase was decanted off
  3. dry with materialdried over magnesium sulfate
  4. customevaporated
  5. customThe residue obtained
  6. customwas recrystallized from ethanol
  7. custom3.3 g (69%) of the expected compound of melting point 155°-156° C. were recovered
  8. filtrationafter filtration
  9. customdrying

出典と根拠

ORDレコード
ord-cd1096d93f37428c9a062b69e3acbaae
出典データセット
uspto-grants-1998_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05709867

反応ノート

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