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HRID 1689276作成日:2026年10月27日
Sodium triacetoxyborohydride → (9-((4-(2-(tert-Butyldimethylsilyloxy)ethyl)thiophen-2-yl)methyl)-1-oxa-4,9-diazaspiro[5.5]undecan-4-yl)(2-isopropylthiazol-4-yl)methanone
https://huagongshe.com/reaction/1689276
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium triacetoxyborohydride | HCID 5049666 | — |
| 反応物 | 3-(2-(Tert-butyldimethylsilyloxy)ethyl)thiophene-2-carbaldehyde | HCID 57988907 | — |
| 反応物 | 4-(2-(Tert-butyldimethylsilyloxy)ethyl)thiophene-2-carbaldehyde | HCID 57989110 | — |
| 反応物 | (2-Isopropylthiazol-4-yl)(1-oxa-4,9-diazaspiro[5.5]undecan-4-yl)methanone trifluoroacetate | HCID 66964182 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 生成物 | (9-((4-(2-(tert-Butyldimethylsilyloxy)ethyl)thiophen-2-yl)methyl)-1-oxa-4,9-diazaspiro[5.5]undecan-4-yl)(2-isopropylthiazol-4-yl)methanone | HCID 57989092 | — |
反応手順
(2-Isopropylthiazol-4-yl)(1-oxa-4,9-diazaspiro[5.5]undecan-4-yl)methanone trifluoroacetate (example 22, step b) (0.50 g) was added to a stirred solution of a 4:1 mixture of 4-(2-(tert-butyldimethylsilyloxy)ethyl)thiophene-2-carbaldehyde and 3-(2-(tert-butyldimethylsilyloxy)ethyl)thiophene-2-carbaldehyde (example 27, step b) (0.40 g) and AcOH (0.085 mL) in N-methyl-2-pyrrolidinone (6 mL). After 5 min, sodium triacetoxyborohydride (0.48 g) was added. After 16 h water was added and the mixture was extracted with ethyl acetate. The ethyl acetate layer was washed three times with water and evaporated in vacuo. Purification by silica gel chromatography eluting with ethyl acetate:isohexane:triethylamine, 20:80:5 separated the two isomeric products and gave the subtitled compound as a gum. Yield 0.27 g.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08148373B2 |
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| 出典データセット | uspto-grants-2012_04 |
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| ORD ID | ord-67e240a48fa64b1ab80639ece1d8bdc6 |
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| 出典メモ | uspto-grants-2012_04 |
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