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氢氧化锂 → HCID 58551346,化合物

HRID 1908158
笔记
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反应方程式

HRID 1908158 反应方程式
[CH2:1]([C:3]1[CH:32]=[CH:31][C:6]([C:7]([N:9]2[CH2:30][CH2:29][C:12]3([C:17]4=[CH:18][CH:19]=[CH:20][N:16]4[C:15]4[CH:21]=[CH:22][C:23]([C:25]([O:27]C)=[O:26])=[CH:24][C:14]=4[O:13]3)[CH2:11][CH2:10]2)=[O:8])=[CH:5][C:4]=1[O:33][CH3:34])[CH3:2].[Li+].[OH-]>O1CCOCC1.C(OCC)(=O)C>[CH2:1]([C:3]1[CH:32]=[CH:31][C:6]([C:7]([N:9]2[CH2:10][CH2:11][C:12]3([O:13][C:14]4[CH:24]=[C:23]([C:25]([OH:27])=[O:26])[CH:22]=[CH:21][C:15]=4[N:16]4[CH:20]=[CH:19][CH:18]=[C:17]34)[CH2:29][CH2:30]2)=[O:8])=[CH:5][C:4]=1[O:33][CH3:34])[CH3:2]
参与物实验过程后处理来源与证据反应笔记

参与物

5

反应物 2

HCID 3939氢氧化锂HCID 58550869HCID 58550869,化合物

产物 1

HCID 58551346HCID 58551346,化合物

试剂、催化剂与溶剂 2

HCID 8857乙酸乙酯溶剂HCID 312751,4-二氧六环溶剂

实验过程

A solution of methyl 1-(4-ethyl-3-methoxy-benzoyl)spiro[piperidine-4,4′-pyrrolo[2,1-c][1,4]benzoxazine]-7′-carboxylate (1.1 g, 2.5 mmol) in LiOH (2.5 mL of 4.0 M, 9.9 mmol) and dioxane (5 mL) was stirred at 50° C. for 1 hour. The reaction was diluted with ethyl acetate and washed with water. The aqueous was acidified with 1N HCl and the product was extracted into ethyl acetate. The organics were dried over sodium sulfate, filtered and evaporated to yield a crude product that was used in the next step without further purification (0.60 g, 53%). ESI-MS m/z calc. 446.5. found 447.5 (M+1)+; Retention time: 1.84 minutes (3 min run).

后处理

  1. washwashed with water
  2. extractionthe product was extracted into ethyl acetate
  3. dry with materialThe organics were dried over sodium sulfate
  4. filtrationfiltered
  5. customevaporated

来源与证据

ORD记录
ord-e79672012de14b68870afc7e13159714
来源数据集
uspto-grants-2013_12
DOI
10.6084/m9.figshare.5104873.v1
专利号
US08598164B2

反应笔记

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本页导航参与物实验过程后处理来源与证据反应笔记