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三乙胺 → HCID 58551320,化合物

HRID 1908159
笔记
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反应方程式

HRID 1908159 反应方程式
[CH2:1]([C:3]1[CH:31]=[CH:30][C:6]([C:7]([N:9]2[CH2:29][CH2:28][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)=[O:26])=[CH:24][C:14]=4[O:13]3)[CH2:11][CH2:10]2)=[O:8])=[CH:5][C:4]=1[O:32][CH3:33])[CH3:2].C(N(CC)CC)C.ClC(OCC(C)C)=O.[BH4-].[Na+]>O1CCCC1.O>[CH2:1]([C:3]1[CH:31]=[CH:30][C:6]([C:7]([N:9]2[CH2:10][CH2:11][C:12]3([O:13][C:14]4[CH:24]=[C:23]([CH2:25][OH:26])[CH:22]=[CH:21][C:15]=4[N:16]4[CH:20]=[CH:19][CH:18]=[C:17]34)[CH2:28][CH2:29]2)=[O:8])=[CH:5][C:4]=1[O:32][CH3:33])[CH3:2]
参与物实验过程后处理来源与证据反应笔记

参与物

7

反应物 4

HCID 8471三乙胺HCID 62365氯甲酸异丁酯HCID 4311764硼氢化钠HCID 58551346HCID 58551346,化合物

产物 1

HCID 58551320HCID 58551320,化合物收率 63.6%

试剂、催化剂与溶剂 2

HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]溶剂
HCID 8028
四氢呋喃
溶剂

实验过程

To 1-(4-ethyl-3-methoxy-benzoyl)spiro[piperidine-4,4′-pyrrolo[2,1-c][1,4]benzoxazine]-7′-carboxylic acid (550 mg, 1.2 mmol) in tetrahydrofuran (2.2 mL) at 0° C. was added triethylamine (200 μL, 1.4 mmol) then isobutyl chloroformate (180 μL, 1.4 mmol). The mixture was stirred for 30 min then filtered. The filtrate was added dropwise to a solution of sodium borohydride (70 mg, 1.8 mmol) in water (770 μL) at 0° C. The mixture was allowed to slowly reach room temperature before it was concentrated to ⅓ volume, diluted with ethyl acetate and washed with 1M HCl. The organics were dried over sodium sulfate, filtered and evaporated to yield (4-ethyl-3-methoxyphenyl)(7-(hydroxymethyl)spiro[benzo[b]pyrrolo[1,2-d][1,4]oxazine-4,4′-piperidine]-1′-yl)methanone (330 mg, 62%). ESI-MS m/z calc. 432.5. found 433.5 (M+1)+; Retention time: 1.78 minutes (3 min run).

后处理

  1. filtrationthen filtered
  2. customwas allowed to slowly reach room temperature before it
  3. concentrationwas concentrated
  4. additiondiluted with ethyl acetate
  5. washwashed with 1M HCl
  6. dry with materialThe organics were dried over sodium sulfate
  7. filtrationfiltered
  8. customevaporated

来源与证据

ORD记录
ord-d480c0a8756b4e0f8bcdbb3f2ebccf5f
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