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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
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Water → HCID 10883437、化合物

HRID 1422067
ノート
印刷プレビュー

反応式

HRID 1422067 の反応式
[CH2:1]([O:8][C:9]1[CH:14]=[CH:13][C:12]([C:15]2[C:16]([CH2:30][CH3:31])=[C:17]3[CH:25]=[CH:24][CH:23]=[C:22]4[N:18]3[C:19]=2[CH:20]=[C:21]4[C:26](OC)=[O:27])=[CH:11][CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-].O.C(=O)([O-])[O-].[K+].[K+]>O1CCCC1.C(OCC)C>[CH2:1]([O:8][C:9]1[CH:10]=[CH:11][C:12]([C:15]2[C:19]3=[CH:20][C:21]([CH2:26][OH:27])=[C:22]4[N:18]3[C:17](=[CH:25][CH:24]=[CH:23]4)[C:16]=2[CH2:30][CH3:31])=[CH:13][CH:14]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
参加物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 962WaterHCID 11430Potassium CarbonateHCID 11144022HCID 11144022、化合物HCID 21226445Aluminium lithium hydride

生成物 1

HCID 10883437HCID 10883437、化合物収率 97%

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒
HCID 8028
Tetrahydrofuran
溶媒

実験手順

Methyl 3-(4-benzyloxyphenyl)-4-ethylpyrrolo[2,1,5-cd]indolizine-1-carboxylate (8.5 g, 20.8 mmol) was dissolved in 170 ml of dry tetrahydrofurane under a nitrogen atmosphere. Lithium aluminium hydride (1.24 g, 32.6 mmol) was added in portions and stirring was continued for 21/2 hours. Water (10 ml) was added dropwise, and 95 ml of saturated aqueous potassium carbonate and 200 ml of diethyl ether was added. The organic layer was separated, and the aqueous layer was extracted with diethyl ether (2×300 ml). The combined organic layers were washed with 200 ml of water and dried over sodium hydrogen carbonate. The solvent was evaporated and the remaining product was dried to afford 7.7 g (97%) of the title compound as yellow crystals. M.p. 148-150° C. MS(SP): m/z 381 (M+). 1H-NMR (CDCl3, 300 MHz) δ: 1.48 (t, 3H); 3.23 (q, 2H); 5,17 (s, 2H); 5.18 (s, 2H); 7.14 (d, 2H); 7.32-7.52 (m, 5H); 7.57 (s, 1H); 7.65 (t, 1H); 7.72 (d, 2H); 7.92 (d, 1H); 8.02 (d, 1H).

後処理

  1. custom2 hours
  2. customThe organic layer was separated
  3. extractionthe aqueous layer was extracted with diethyl ether (2×300 ml)
  4. washThe combined organic layers were washed with 200 ml of water
  5. dry with materialdried over sodium hydrogen carbonate
  6. customThe solvent was evaporated
  7. customthe remaining product was dried

出典と根拠

ORDレコード
ord-2f1153f346d741378f5230c22571cf97
出典データセット
uspto-grants-2000_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06080754

反応ノート

読み込み中…

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